# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_H3L _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 O8' _chemical_formula_sum 'C24 H22 O8' _chemical_formula_weight 438.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 42.4912(6) _cell_length_b 12.0468(15) _cell_length_c 17.2900(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8850.5(12) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3549 _cell_measurement_theta_min 3.0319 _cell_measurement_theta_max 29.1282 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9632 _exptl_absorpt_correction_T_max 0.9718 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8339 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3774 _reflns_number_gt 3335 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For C23, C24, O1 and O1', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+6.2114P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(11) _refine_ls_number_reflns 3774 _refine_ls_number_parameters 301 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.90993(5) -0.1146(2) 0.89180(14) 0.0440(6) Uani 1 1 d . . . C2 C -0.91411(6) -0.2254(2) 0.87122(15) 0.0460(6) Uani 1 1 d . . . H2 H -0.9343 -0.2549 0.8679 0.055 Uiso 1 1 calc R . . C3 C -0.88833(5) -0.2913(2) 0.85572(13) 0.0414(5) Uani 1 1 d . . . C4 C -0.85782(5) -0.2480(2) 0.86154(14) 0.0440(6) Uani 1 1 d . . . H4 H -0.8405 -0.2925 0.8508 0.053 Uiso 1 1 calc R . . C5 C -0.85376(5) -0.1384(2) 0.88349(14) 0.0424(6) Uani 1 1 d . . . C6 C -0.87993(5) -0.0714(2) 0.89768(15) 0.0454(6) Uani 1 1 d . . . H6 H -0.8771 0.0027 0.9111 0.055 Uiso 1 1 calc R . . C7 C -0.93777(6) -0.0419(3) 0.90419(17) 0.0546(7) Uani 1 1 d . . . C8 C -0.89200(6) -0.4096(2) 0.83244(14) 0.0446(6) Uani 1 1 d . . . C9 C -0.79758(5) -0.1533(2) 0.88449(18) 0.0519(7) Uani 1 1 d . . . H9A H -0.7960 -0.1830 0.8325 0.062 Uiso 1 1 calc R . . H9B H -0.7985 -0.2149 0.9205 0.062 Uiso 1 1 calc R . . C10 C -0.76932(5) -0.0810(2) 0.90212(15) 0.0447(6) Uani 1 1 d . . . C11 C -0.74199(5) -0.0951(2) 0.85885(16) 0.0477(6) Uani 1 1 d . . . H11 H -0.7416 -0.1461 0.8185 0.057 Uiso 1 1 calc R . . C12 C -0.71551(6) -0.0333(2) 0.87570(16) 0.0486(6) Uani 1 1 d . . . H12 H -0.6974 -0.0437 0.8465 0.058 Uiso 1 1 calc R . . C13 C -0.71532(5) 0.0437(2) 0.93512(14) 0.0412(5) Uani 1 1 d . . . C14 C -0.74282(6) 0.0596(2) 0.97659(17) 0.0537(7) Uani 1 1 d . . . H14 H -0.7435 0.1127 1.0156 0.064 Uiso 1 1 calc R . . C15 C -0.76942(6) -0.0031(3) 0.96034(16) 0.0570(7) Uani 1 1 d . . . H15 H -0.7876 0.0077 0.9893 0.068 Uiso 1 1 calc R . . C16 C -0.68689(5) 0.1146(2) 0.94894(14) 0.0409(5) Uani 1 1 d . . . C17 C -0.65803(5) 0.0756(2) 0.97766(13) 0.0391(5) Uani 1 1 d . . . C18 C -0.63233(6) 0.1471(2) 0.98043(15) 0.0485(6) Uani 1 1 d . . . H18 H -0.6131 0.1206 0.9980 0.058 Uiso 1 1 calc R . . C19 C -0.63478(6) 0.2559(2) 0.95777(17) 0.0568(7) Uani 1 1 d . . . H19 H -0.6173 0.3023 0.9598 0.068 Uiso 1 1 calc R . . C20 C -0.66332(7) 0.2960(3) 0.9320(2) 0.0634(8) Uani 1 1 d . . . H20 H -0.6653 0.3701 0.9176 0.076 Uiso 1 1 calc R . . C21 C -0.68878(6) 0.2261(2) 0.92776(18) 0.0573(7) Uani 1 1 d . . . H21 H -0.7079 0.2540 0.9102 0.069 Uiso 1 1 calc R . . C22 C -0.65415(6) -0.0398(2) 1.00724(14) 0.0412(6) Uani 1 1 d . . . C23 C -0.79003(15) 0.1023(6) 0.7210(4) 0.150(2) Uani 1 1 d U . . H23A H -0.7872 0.1813 0.7201 0.225 Uiso 1 1 calc R . . H23B H -0.7897 0.0765 0.7735 0.225 Uiso 1 1 calc R . . H23C H -0.8099 0.0837 0.6979 0.225 Uiso 1 1 calc R . . C24 C -0.76602(11) 0.0523(4) 0.6800(3) 0.1075(14) Uani 1 1 d U . . H24A H -0.7459 0.0719 0.7028 0.129 Uiso 1 1 calc R . . H24B H -0.7662 0.0788 0.6270 0.129 Uiso 1 1 calc R . . O1 O -0.96387(10) -0.0804(4) 0.9210(3) 0.0576(11) Uani 0.50 1 d PU . . O1' O -0.96471(9) -0.0730(4) 0.8849(3) 0.0544(11) Uani 0.50 1 d PU . . O2 O -0.93123(4) 0.06247(18) 0.91742(14) 0.0705(6) Uani 1 1 d . . . H2' H -0.9476 0.0987 0.9177 0.106 Uiso 1 1 calc R . . O3 O -0.92095(4) -0.44432(17) 0.82756(14) 0.0652(6) Uani 1 1 d . . . H3' H -0.9211 -0.5098 0.8145 0.098 Uiso 1 1 calc R . . O4 O -0.86888(4) -0.46910(16) 0.81819(11) 0.0520(4) Uani 1 1 d . . . O5 O -0.82531(4) -0.08600(15) 0.89150(13) 0.0577(5) Uani 1 1 d . . . O6 O -0.67627(4) -0.09960(17) 1.02513(13) 0.0617(5) Uani 1 1 d . . . O7 O -0.62477(4) -0.07242(17) 1.01317(11) 0.0566(5) Uani 1 1 d . . . H7' H -0.6243 -0.1361 1.0299 0.085 Uiso 1 1 calc R . . O8 O -0.76970(5) -0.06366(19) 0.68079(16) 0.0759(6) Uani 1 1 d . . . H8 H -0.7534 -0.0932 0.6658 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0342(12) 0.0435(14) 0.0544(14) -0.0008(11) -0.0038(10) -0.0028(11) C2 0.0313(12) 0.0490(15) 0.0578(14) 0.0017(12) -0.0074(10) -0.0094(11) C3 0.0401(13) 0.0376(13) 0.0465(12) 0.0030(10) -0.0071(10) -0.0051(11) C4 0.0309(12) 0.0406(15) 0.0605(14) 0.0005(11) -0.0014(10) -0.0011(10) C5 0.0318(11) 0.0383(14) 0.0572(14) 0.0019(11) -0.0042(10) -0.0071(10) C6 0.0363(12) 0.0368(14) 0.0632(15) 0.0001(11) -0.0060(11) -0.0061(11) C7 0.0309(12) 0.0515(17) 0.0814(18) -0.0031(14) -0.0014(12) -0.0068(12) C8 0.0387(13) 0.0428(15) 0.0523(14) 0.0007(12) -0.0107(10) -0.0071(12) C9 0.0302(12) 0.0416(15) 0.0839(19) -0.0004(13) -0.0043(12) -0.0013(10) C10 0.0334(12) 0.0401(14) 0.0605(15) 0.0047(12) -0.0050(10) -0.0010(10) C11 0.0354(13) 0.0368(14) 0.0708(16) -0.0064(12) -0.0008(11) 0.0029(11) C12 0.0321(12) 0.0431(14) 0.0705(16) -0.0003(13) 0.0044(11) 0.0020(11) C13 0.0330(12) 0.0357(13) 0.0550(14) 0.0060(11) -0.0046(10) 0.0005(10) C14 0.0391(14) 0.0605(18) 0.0616(15) -0.0119(13) 0.0024(11) -0.0038(13) C15 0.0367(14) 0.0672(19) 0.0672(17) -0.0080(15) 0.0090(12) -0.0069(13) C16 0.0367(12) 0.0329(13) 0.0530(13) 0.0027(10) 0.0004(10) -0.0044(11) C17 0.0348(12) 0.0354(13) 0.0472(12) -0.0039(10) 0.0006(10) -0.0007(10) C18 0.0372(13) 0.0482(15) 0.0600(14) -0.0029(12) -0.0048(11) -0.0058(12) C19 0.0474(15) 0.0439(16) 0.0790(19) -0.0005(13) -0.0035(13) -0.0163(13) C20 0.0556(16) 0.0370(15) 0.098(2) 0.0106(15) -0.0003(15) -0.0088(13) C21 0.0434(14) 0.0425(16) 0.086(2) 0.0140(14) -0.0074(13) -0.0003(13) C22 0.0349(13) 0.0389(14) 0.0499(13) -0.0002(11) -0.0043(10) 0.0010(11) C23 0.151(2) 0.149(2) 0.150(2) 0.0008(10) 0.0017(10) 0.0023(10) C24 0.1076(16) 0.1061(16) 0.1088(16) -0.0018(10) 0.0005(10) 0.0007(10) O1 0.0534(14) 0.0599(14) 0.0596(14) 0.0012(10) 0.0024(10) -0.0021(9) O1' 0.0498(13) 0.0566(14) 0.0566(13) -0.0009(10) -0.0013(9) -0.0009(9) O2 0.0422(10) 0.0525(13) 0.1168(18) -0.0174(12) -0.0032(11) 0.0021(9) O3 0.0430(10) 0.0474(12) 0.1053(15) -0.0164(11) -0.0059(10) -0.0117(9) O4 0.0441(10) 0.0443(10) 0.0675(11) -0.0060(9) -0.0067(8) -0.0016(9) O5 0.0291(8) 0.0388(10) 0.1054(15) -0.0071(10) -0.0056(9) -0.0038(7) O6 0.0416(10) 0.0492(12) 0.0942(14) 0.0212(11) -0.0011(9) -0.0003(9) O7 0.0429(10) 0.0468(11) 0.0800(12) 0.0077(9) -0.0081(8) 0.0058(9) O8 0.0542(12) 0.0613(14) 0.1123(18) -0.0122(13) 0.0003(12) -0.0042(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.381(3) . ? C1 C2 1.392(4) . ? C1 C7 1.488(4) . ? C2 C3 1.379(4) . ? C2 H2 0.9300 . ? C3 C4 1.401(3) . ? C3 C8 1.489(4) . ? C4 C5 1.385(4) . ? C4 H4 0.9300 . ? C5 O5 1.371(3) . ? C5 C6 1.396(3) . ? C6 H6 0.9300 . ? C7 O1 1.237(5) . ? C7 O1' 1.250(5) . ? C7 O2 1.307(4) . ? C8 O4 1.241(3) . ? C8 O3 1.302(3) . ? C9 O5 1.435(3) . ? C9 C10 1.514(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.376(4) . ? C10 C11 1.392(4) . ? C11 C12 1.380(3) . ? C11 H11 0.9300 . ? C12 C13 1.384(4) . ? C12 H12 0.9300 . ? C13 C14 1.384(3) . ? C13 C16 1.498(3) . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.395(4) . ? C16 C17 1.404(3) . ? C17 C18 1.392(3) . ? C17 C22 1.490(3) . ? C18 C19 1.371(4) . ? C18 H18 0.9300 . ? C19 C20 1.380(4) . ? C19 H19 0.9300 . ? C20 C21 1.373(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 O6 1.224(3) . ? C22 O7 1.313(3) . ? C23 C24 1.381(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O8 1.405(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? O1 O1' 0.631(4) . ? O2 H2' 0.8200 . ? O3 H3' 0.8200 . ? O7 H7' 0.8200 . ? O8 H8 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.9(2) . . ? C6 C1 C7 120.1(2) . . ? C2 C1 C7 120.0(2) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.5(2) . . ? C2 C3 C8 121.3(2) . . ? C4 C3 C8 118.2(2) . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? O5 C5 C4 125.2(2) . . ? O5 C5 C6 114.7(2) . . ? C4 C5 C6 120.0(2) . . ? C1 C6 C5 120.3(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? O1 C7 O1' 29.4(2) . . ? O1 C7 O2 120.7(3) . . ? O1' C7 O2 122.0(3) . . ? O1 C7 C1 121.7(3) . . ? O1' C7 C1 120.9(3) . . ? O2 C7 C1 115.0(2) . . ? O4 C8 O3 123.3(2) . . ? O4 C8 C3 121.6(2) . . ? O3 C8 C3 115.1(2) . . ? O5 C9 C10 108.0(2) . . ? O5 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? O5 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C15 C10 C11 118.6(2) . . ? C15 C10 C9 122.5(2) . . ? C11 C10 C9 118.9(2) . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.5(2) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 118.2(2) . . ? C14 C13 C16 121.3(2) . . ? C12 C13 C16 120.3(2) . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 121.1(2) . . ? C10 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C21 C16 C17 117.7(2) . . ? C21 C16 C13 117.4(2) . . ? C17 C16 C13 124.8(2) . . ? C18 C17 C16 119.3(2) . . ? C18 C17 C22 118.6(2) . . ? C16 C17 C22 122.0(2) . . ? C19 C18 C17 121.5(2) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 119.6(2) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 119.7(3) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C16 122.1(3) . . ? C20 C21 H21 118.9 . . ? C16 C21 H21 118.9 . . ? O6 C22 O7 122.3(2) . . ? O6 C22 C17 123.4(2) . . ? O7 C22 C17 114.3(2) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C24 O8 110.2(5) . . ? C23 C24 H24A 109.6 . . ? O8 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? O8 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? O1' O1 C7 76.4(6) . . ? O1 O1' C7 74.2(6) . . ? C7 O2 H2' 109.5 . . ? C8 O3 H3' 109.5 . . ? C5 O5 C9 117.10(19) . . ? C22 O7 H7' 109.5 . . ? C24 O8 H8 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.9(4) . . . . ? C7 C1 C2 C3 176.5(2) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C1 C2 C3 C8 -179.1(2) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C8 C3 C4 C5 -179.7(2) . . . . ? C3 C4 C5 O5 179.9(2) . . . . ? C3 C4 C5 C6 -1.6(3) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? C7 C1 C6 C5 -177.8(2) . . . . ? O5 C5 C6 C1 -179.7(2) . . . . ? C4 C5 C6 C1 1.6(4) . . . . ? C6 C1 C7 O1 -159.3(4) . . . . ? C2 C1 C7 O1 23.3(5) . . . . ? C6 C1 C7 O1' 166.2(3) . . . . ? C2 C1 C7 O1' -11.3(5) . . . . ? C6 C1 C7 O2 2.5(4) . . . . ? C2 C1 C7 O2 -174.9(3) . . . . ? C2 C3 C8 O4 179.8(2) . . . . ? C4 C3 C8 O4 -0.2(3) . . . . ? C2 C3 C8 O3 0.5(3) . . . . ? C4 C3 C8 O3 -179.5(2) . . . . ? O5 C9 C10 C15 39.9(4) . . . . ? O5 C9 C10 C11 -141.3(2) . . . . ? C15 C10 C11 C12 1.4(4) . . . . ? C9 C10 C11 C12 -177.5(2) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C11 C12 C13 C14 -1.5(4) . . . . ? C11 C12 C13 C16 -176.2(2) . . . . ? C12 C13 C14 C15 2.2(4) . . . . ? C16 C13 C14 C15 176.8(2) . . . . ? C11 C10 C15 C14 -0.7(4) . . . . ? C9 C10 C15 C14 178.1(3) . . . . ? C13 C14 C15 C10 -1.1(5) . . . . ? C14 C13 C16 C21 -68.0(3) . . . . ? C12 C13 C16 C21 106.5(3) . . . . ? C14 C13 C16 C17 115.7(3) . . . . ? C12 C13 C16 C17 -69.8(3) . . . . ? C21 C16 C17 C18 -3.0(4) . . . . ? C13 C16 C17 C18 173.3(2) . . . . ? C21 C16 C17 C22 175.5(2) . . . . ? C13 C16 C17 C22 -8.2(4) . . . . ? C16 C17 C18 C19 1.9(4) . . . . ? C22 C17 C18 C19 -176.7(3) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C18 C19 C20 C21 -1.4(5) . . . . ? C19 C20 C21 C16 0.2(5) . . . . ? C17 C16 C21 C20 2.1(4) . . . . ? C13 C16 C21 C20 -174.6(3) . . . . ? C18 C17 C22 O6 161.4(3) . . . . ? C16 C17 C22 O6 -17.1(4) . . . . ? C18 C17 C22 O7 -18.2(3) . . . . ? C16 C17 C22 O7 163.3(2) . . . . ? O2 C7 O1 O1' 101.6(7) . . . . ? C1 C7 O1 O1' -97.6(7) . . . . ? O2 C7 O1' O1 -96.8(7) . . . . ? C1 C7 O1' O1 100.7(7) . . . . ? C4 C5 O5 C9 -6.9(4) . . . . ? C6 C5 O5 C9 174.5(2) . . . . ? C10 C9 O5 C5 -175.2(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2' O8 0.82 1.76 2.575(3) 171.4 3_355 O3 H3' O6 0.82 1.84 2.652(3) 171.2 12_444 O7 H7' O4 0.82 1.88 2.697(3) 174.5 4_545 O8 H8 O1 0.82 1.92 2.699(5) 158.8 8_544 O8 H8 O1' 0.82 2.00 2.820(5) 174.9 8_544 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.204 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.034 _database_code_depnum_ccdc_archive 'CCDC 938332' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H31 Na O19 Zn5' _chemical_formula_sum 'C44 H31 Na O19 Zn5' _chemical_formula_weight 1213.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3320(9) _cell_length_b 13.7920(11) _cell_length_c 17.3310(14) _cell_angle_alpha 70.708(7) _cell_angle_beta 88.355(7) _cell_angle_gamma 87.483(7) _cell_volume 2328.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3333 _cell_measurement_theta_min 3.1255 _cell_measurement_theta_max 29.1625 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 2.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5387 _exptl_absorpt_correction_T_max 0.5846 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18085 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8057 _reflns_number_gt 5130 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8057 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.72801(7) 0.25007(7) 0.50817(5) 0.0377(2) Uani 1 1 d . . . Zn2 Zn 0.56806(7) 0.17860(6) 0.37224(4) 0.0331(2) Uani 1 1 d . . . Zn3 Zn 0.38065(7) 0.14920(6) 0.24617(5) 0.0348(2) Uani 1 1 d . . . Zn4 Zn 0.55098(7) 0.04300(6) 0.56625(4) 0.0323(2) Uani 1 1 d . . . Zn5 Zn -0.25746(7) 0.08446(7) 0.70936(5) 0.0376(2) Uani 1 1 d . . . C1 C 0.3477(6) 0.1469(5) 0.7453(4) 0.0311(15) Uani 1 1 d . . . C2 C 0.2295(6) 0.1192(5) 0.7223(4) 0.0315(15) Uani 1 1 d . . . H2 H 0.2295 0.0817 0.6865 0.038 Uiso 1 1 calc R . . C3 C 0.1133(6) 0.1468(5) 0.7521(4) 0.0327(16) Uani 1 1 d . . . C4 C 0.1136(6) 0.2047(6) 0.8055(4) 0.0369(17) Uani 1 1 d . . . H4 H 0.0359 0.2253 0.8249 0.044 Uiso 1 1 calc R . . C5 C 0.2307(6) 0.2306(6) 0.8289(4) 0.0403(18) Uani 1 1 d . . . C6 C 0.3459(6) 0.2036(6) 0.7984(4) 0.0396(18) Uani 1 1 d . . . H6 H 0.4235 0.2236 0.8134 0.047 Uiso 1 1 calc R . . C7 C 0.4718(6) 0.1155(5) 0.7141(4) 0.0315(16) Uani 1 1 d . . . C8 C -0.0126(6) 0.1168(6) 0.7259(4) 0.0371(17) Uani 1 1 d . . . C9 C 0.3423(7) 0.3169(7) 0.9031(5) 0.053(2) Uani 1 1 d . . . H9A H 0.3820 0.3639 0.8545 0.064 Uiso 1 1 calc R . . H9B H 0.4006 0.2573 0.9241 0.064 Uiso 1 1 calc R . . C10 C 0.3206(7) 0.3689(6) 0.9666(4) 0.0453(19) Uani 1 1 d . . . C11 C 0.2091(7) 0.4213(6) 0.9770(4) 0.0468(19) Uani 1 1 d . . . H11 H 0.1374 0.4238 0.9451 0.056 Uiso 1 1 calc R . . C12 C 0.2036(7) 0.4707(6) 1.0356(4) 0.0461(19) Uani 1 1 d . . . H12 H 0.1290 0.5088 1.0404 0.055 Uiso 1 1 calc R . . C13 C 0.3053(7) 0.4645(5) 1.0862(4) 0.0343(16) Uani 1 1 d . . . C14 C 0.4183(7) 0.4119(6) 1.0731(4) 0.048(2) Uani 1 1 d . . . H14 H 0.4906 0.4099 1.1044 0.058 Uiso 1 1 calc R . . C15 C 0.4260(7) 0.3637(6) 1.0163(4) 0.050(2) Uani 1 1 d . . . H15 H 0.5015 0.3272 1.0105 0.060 Uiso 1 1 calc R . . C16 C 0.3009(6) 0.5130(5) 1.1520(4) 0.0351(16) Uani 1 1 d . . . C17 C 0.2618(8) 0.6157(6) 1.1319(5) 0.052(2) Uani 1 1 d . . . H17 H 0.2330 0.6510 1.0794 0.063 Uiso 1 1 calc R . . C18 C 0.2646(10) 0.6665(7) 1.1883(6) 0.077(3) Uani 1 1 d . . . H18 H 0.2390 0.7356 1.1737 0.092 Uiso 1 1 calc R . . C19 C 0.3059(10) 0.6136(8) 1.2665(6) 0.076(3) Uani 1 1 d . . . H19 H 0.3034 0.6458 1.3060 0.091 Uiso 1 1 calc R . . C20 C 0.3505(9) 0.5138(7) 1.2859(5) 0.067(3) Uani 1 1 d . . . H20 H 0.3833 0.4800 1.3377 0.080 Uiso 1 1 calc R . . C21 C 0.3477(6) 0.4616(5) 1.2293(4) 0.0353(16) Uani 1 1 d . . . C22 C 0.3857(6) 0.3490(6) 1.2579(4) 0.0349(16) Uani 1 1 d . . . C23 C 1.3370(6) 0.3164(5) 0.5353(4) 0.0326(16) Uani 1 1 d . . . C24 C 1.2242(6) 0.2818(5) 0.5127(4) 0.0341(16) Uani 1 1 d . . . H24 H 1.2296 0.2363 0.4832 0.041 Uiso 1 1 calc R . . C25 C 1.1060(6) 0.3142(5) 0.5335(4) 0.0319(16) Uani 1 1 d . . . C26 C 1.0966(6) 0.3815(5) 0.5775(4) 0.0379(17) Uani 1 1 d . . . H26 H 1.0155 0.4041 0.5906 0.045 Uiso 1 1 calc R . . C27 C 1.2070(6) 0.4153(5) 0.6021(4) 0.0373(17) Uani 1 1 d . . . C28 C 1.3272(6) 0.3832(6) 0.5803(4) 0.0399(18) Uani 1 1 d . . . H28 H 1.4019 0.4066 0.5959 0.048 Uiso 1 1 calc R . . C29 C 1.4673(6) 0.2735(5) 0.5181(4) 0.0333(16) Uani 1 1 d . . . C30 C 0.9822(7) 0.2753(6) 0.5116(4) 0.0403(18) Uani 1 1 d . . . C31 C 1.0873(7) 0.4957(6) 0.6836(5) 0.047(2) Uani 1 1 d . . . H31A H 1.0543 0.4304 0.7177 0.056 Uiso 1 1 calc R . . H31B H 1.0248 0.5278 0.6412 0.056 Uiso 1 1 calc R . . C32 C 1.1046(7) 0.5634(6) 0.7342(4) 0.0413(18) Uani 1 1 d . . . C33 C 0.9978(7) 0.6181(7) 0.7514(6) 0.066(3) Uani 1 1 d . . . H33 H 0.9175 0.6125 0.7306 0.080 Uiso 1 1 calc R . . C34 C 1.0081(7) 0.6796(7) 0.7980(6) 0.064(3) Uani 1 1 d . . . H34 H 0.9339 0.7113 0.8117 0.077 Uiso 1 1 calc R . . C35 C 1.1290(7) 0.6962(6) 0.8259(4) 0.0437(19) Uani 1 1 d . . . C36 C 1.2320(7) 0.6390(6) 0.8113(4) 0.0404(18) Uani 1 1 d . . . H36 H 1.3125 0.6444 0.8319 0.048 Uiso 1 1 calc R . . C37 C 1.2202(7) 0.5726(6) 0.7665(4) 0.0444(18) Uani 1 1 d . . . H37 H 1.2923 0.5341 0.7585 0.053 Uiso 1 1 calc R . . C38 C 1.1398(7) 0.7698(6) 0.8713(4) 0.0431(18) Uani 1 1 d . . . C39 C 1.0463(8) 0.7746(7) 0.9278(5) 0.064(2) Uani 1 1 d . . . H39 H 0.9762 0.7320 0.9364 0.077 Uiso 1 1 calc R . . C40 C 1.0528(9) 0.8405(9) 0.9724(6) 0.079(3) Uani 1 1 d . . . H40 H 0.9880 0.8417 1.0104 0.095 Uiso 1 1 calc R . . C41 C 1.1533(10) 0.9032(7) 0.9607(5) 0.069(3) Uani 1 1 d . . . H41 H 1.1567 0.9489 0.9898 0.082 Uiso 1 1 calc R . . C42 C 1.2499(8) 0.8995(6) 0.9062(5) 0.054(2) Uani 1 1 d . . . H42 H 1.3217 0.9396 0.9011 0.065 Uiso 1 1 calc R . . C43 C 1.2429(7) 0.8372(6) 0.8583(4) 0.0387(17) Uani 1 1 d . . . C44 C 1.3486(7) 0.8430(5) 0.7959(4) 0.0413(18) Uani 1 1 d . . . O1 O 0.5755(4) 0.1400(4) 0.7380(3) 0.0417(12) Uani 1 1 d . . . O2 O 0.4648(4) 0.0669(4) 0.6666(3) 0.0441(13) Uani 1 1 d . . . O3 O -0.0103(5) 0.0635(5) 0.6800(4) 0.0647(17) Uani 1 1 d . . . O4 O -0.1166(4) 0.1459(4) 0.7515(3) 0.0477(13) Uani 1 1 d . . . O5 O 0.2228(4) 0.2858(5) 0.8829(3) 0.0615(17) Uani 1 1 d . . . O6 O 0.3143(4) 0.2903(4) 1.2357(3) 0.0428(12) Uani 1 1 d . . . O7 O 0.4851(4) 0.3191(4) 1.3004(3) 0.0391(12) Uani 1 1 d . . . O8 O 0.8783(4) 0.3131(4) 0.5301(3) 0.0436(12) Uani 1 1 d . . . O9 O 0.9887(5) 0.2078(5) 0.4780(4) 0.0671(17) Uani 1 1 d . . . O10 O 1.4711(4) 0.1981(4) 0.4919(3) 0.0400(12) Uani 1 1 d . . . O11 O 1.5658(4) 0.3139(4) 0.5341(3) 0.0468(13) Uani 1 1 d . . . O12 O 1.2062(4) 0.4792(4) 0.6478(3) 0.0515(14) Uani 1 1 d . . . O13 O 1.3198(4) 0.8490(4) 0.7247(3) 0.0402(12) Uani 1 1 d . . . O14 O 1.4632(5) 0.8440(4) 0.8202(3) 0.0461(13) Uani 1 1 d . . . O15 O 0.7275(4) 0.1064(3) 0.5887(3) 0.0343(11) Uani 1 1 d . . . O16 O 0.6124(4) 0.0331(3) 0.4568(3) 0.0354(11) Uani 1 1 d . . . O17 O 0.7188(4) 0.2443(4) 0.3989(3) 0.0485(14) Uani 1 1 d . . . O18 O 0.3998(4) 0.1058(3) 0.3654(2) 0.0335(11) Uani 1 1 d . . . O19 O 0.2556(4) 0.0630(4) 0.2254(3) 0.0445(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0234(4) 0.0525(6) 0.0457(5) -0.0268(4) -0.0034(3) -0.0078(4) Zn2 0.0272(4) 0.0422(5) 0.0338(4) -0.0170(4) -0.0053(3) -0.0051(4) Zn3 0.0343(4) 0.0380(5) 0.0373(4) -0.0185(4) -0.0050(3) -0.0052(4) Zn4 0.0352(4) 0.0351(5) 0.0325(4) -0.0188(4) 0.0010(3) -0.0043(4) Zn5 0.0270(4) 0.0482(6) 0.0465(5) -0.0271(4) -0.0042(3) -0.0042(4) C1 0.026(3) 0.035(4) 0.036(4) -0.016(3) -0.004(3) -0.002(3) C2 0.026(4) 0.036(4) 0.040(4) -0.022(3) 0.004(3) -0.003(3) C3 0.023(3) 0.037(4) 0.042(4) -0.017(3) 0.003(3) -0.006(3) C4 0.020(3) 0.056(5) 0.041(4) -0.025(4) 0.003(3) 0.003(3) C5 0.027(4) 0.055(5) 0.052(4) -0.035(4) 0.006(3) -0.002(3) C6 0.027(4) 0.053(5) 0.049(4) -0.030(4) -0.007(3) -0.003(3) C7 0.026(4) 0.036(4) 0.036(4) -0.017(3) 0.001(3) -0.004(3) C8 0.017(4) 0.046(5) 0.050(4) -0.018(4) -0.004(3) 0.004(3) C9 0.047(5) 0.076(6) 0.055(5) -0.045(5) -0.008(4) -0.006(4) C10 0.055(5) 0.040(5) 0.048(4) -0.022(4) -0.008(4) -0.007(4) C11 0.041(4) 0.057(5) 0.046(4) -0.022(4) -0.011(3) 0.001(4) C12 0.047(5) 0.043(5) 0.050(5) -0.019(4) -0.003(4) 0.008(4) C13 0.046(4) 0.027(4) 0.030(4) -0.008(3) -0.002(3) -0.006(3) C14 0.041(4) 0.059(5) 0.053(5) -0.030(4) -0.007(4) 0.004(4) C15 0.045(5) 0.063(6) 0.052(5) -0.037(5) 0.004(4) 0.005(4) C16 0.031(4) 0.027(4) 0.052(4) -0.020(4) -0.006(3) 0.006(3) C17 0.068(5) 0.044(5) 0.051(5) -0.025(4) -0.017(4) 0.009(4) C18 0.104(8) 0.048(6) 0.093(7) -0.045(6) -0.021(6) 0.029(5) C19 0.103(8) 0.058(7) 0.086(7) -0.051(6) -0.011(6) 0.017(6) C20 0.082(6) 0.067(7) 0.066(6) -0.040(5) -0.028(5) 0.016(5) C21 0.033(4) 0.032(4) 0.046(4) -0.022(4) -0.006(3) 0.010(3) C22 0.029(4) 0.046(5) 0.032(4) -0.016(4) -0.004(3) 0.004(3) C23 0.023(3) 0.036(4) 0.046(4) -0.023(4) -0.007(3) -0.002(3) C24 0.031(4) 0.033(4) 0.041(4) -0.015(3) 0.000(3) -0.002(3) C25 0.026(4) 0.036(4) 0.039(4) -0.021(3) 0.001(3) -0.004(3) C26 0.027(4) 0.040(4) 0.051(4) -0.020(4) 0.001(3) -0.006(3) C27 0.030(4) 0.044(5) 0.050(4) -0.031(4) -0.001(3) -0.006(3) C28 0.018(3) 0.057(5) 0.057(4) -0.034(4) -0.010(3) -0.002(3) C29 0.027(4) 0.040(4) 0.036(4) -0.015(3) -0.005(3) -0.005(3) C30 0.027(4) 0.050(5) 0.053(4) -0.030(4) -0.010(3) 0.002(3) C31 0.038(4) 0.051(5) 0.065(5) -0.036(4) 0.009(4) -0.008(4) C32 0.033(4) 0.040(5) 0.057(5) -0.023(4) 0.017(3) -0.014(3) C33 0.034(5) 0.096(7) 0.100(7) -0.075(6) 0.000(4) -0.003(4) C34 0.028(4) 0.092(7) 0.098(7) -0.065(6) 0.003(4) -0.001(4) C35 0.042(4) 0.052(5) 0.047(4) -0.029(4) 0.013(3) -0.008(4) C36 0.039(4) 0.048(5) 0.035(4) -0.015(4) -0.002(3) -0.003(4) C37 0.041(4) 0.041(5) 0.056(5) -0.024(4) -0.005(3) 0.008(3) C38 0.042(4) 0.052(5) 0.042(4) -0.025(4) 0.014(3) -0.005(4) C39 0.062(6) 0.070(6) 0.072(6) -0.040(5) 0.024(5) -0.013(5) C40 0.074(7) 0.110(9) 0.077(7) -0.062(7) 0.033(5) -0.017(6) C41 0.101(8) 0.068(7) 0.054(5) -0.044(5) 0.020(5) -0.013(6) C42 0.062(5) 0.058(6) 0.053(5) -0.034(5) 0.013(4) -0.004(4) C43 0.043(4) 0.045(5) 0.032(4) -0.018(4) 0.003(3) 0.001(3) C44 0.054(5) 0.029(4) 0.042(4) -0.015(4) 0.008(4) -0.002(3) O1 0.015(2) 0.065(4) 0.056(3) -0.035(3) 0.001(2) -0.002(2) O2 0.029(3) 0.058(3) 0.060(3) -0.040(3) 0.013(2) -0.011(2) O3 0.044(3) 0.090(5) 0.091(4) -0.069(4) -0.007(3) -0.010(3) O4 0.018(3) 0.058(4) 0.083(4) -0.045(3) -0.006(2) -0.003(2) O5 0.029(3) 0.108(5) 0.085(4) -0.082(4) 0.006(2) -0.008(3) O6 0.045(3) 0.039(3) 0.048(3) -0.019(3) -0.014(2) -0.004(2) O7 0.035(3) 0.037(3) 0.043(3) -0.010(2) -0.011(2) -0.004(2) O8 0.021(3) 0.052(3) 0.069(3) -0.035(3) -0.002(2) -0.005(2) O9 0.045(3) 0.084(5) 0.105(5) -0.074(4) -0.014(3) -0.005(3) O10 0.024(2) 0.041(3) 0.063(3) -0.030(3) -0.002(2) 0.006(2) O11 0.025(3) 0.056(3) 0.071(3) -0.036(3) -0.005(2) 0.000(2) O12 0.025(3) 0.064(4) 0.088(4) -0.056(3) 0.007(2) -0.008(2) O13 0.039(3) 0.047(3) 0.038(3) -0.021(2) 0.007(2) 0.000(2) O14 0.039(3) 0.053(3) 0.048(3) -0.019(3) 0.003(2) -0.004(2) O15 0.029(2) 0.043(3) 0.042(3) -0.028(2) -0.0034(19) -0.004(2) O16 0.042(3) 0.037(3) 0.033(2) -0.020(2) -0.0015(19) 0.001(2) O17 0.041(3) 0.073(4) 0.036(3) -0.021(3) -0.008(2) -0.027(3) O18 0.031(2) 0.037(3) 0.034(2) -0.013(2) -0.0028(19) -0.005(2) O19 0.040(3) 0.040(3) 0.055(3) -0.017(3) -0.013(2) -0.010(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O8 1.919(4) . ? Zn1 O17 1.926(4) . ? Zn1 O11 1.968(5) 1_455 ? Zn1 O15 2.012(5) . ? Zn2 O17 1.975(4) . ? Zn2 O18 2.071(4) . ? Zn2 O7 2.088(5) 1_554 ? Zn2 O16 2.098(5) . ? Zn2 O13 2.140(4) 2_766 ? Zn2 O10 2.367(5) 1_455 ? Zn2 Zn3 3.0959(9) . ? Zn3 O19 1.912(4) . ? Zn3 O14 1.942(5) 2_766 ? Zn3 O18 1.965(4) . ? Zn3 O6 1.987(5) 1_554 ? Zn4 O16 2.028(4) . ? Zn4 O2 2.047(4) . ? Zn4 O18 2.052(5) 2_656 ? Zn4 O16 2.141(4) 2_656 ? Zn4 O15 2.156(4) . ? Zn4 O10 2.237(5) 1_455 ? Zn4 Zn4 3.1365(13) 2_656 ? Zn5 O19 1.972(5) 2_556 ? Zn5 O1 1.974(4) 1_455 ? Zn5 O4 1.987(4) . ? Zn5 O15 2.020(4) 1_455 ? C1 C6 1.390(9) . ? C1 C2 1.402(8) . ? C1 C7 1.480(9) . ? C2 C3 1.381(9) . ? C2 H2 0.9300 . ? C3 C4 1.409(9) . ? C3 C8 1.507(8) . ? C4 C5 1.386(8) . ? C4 H4 0.9300 . ? C5 C6 1.374(9) . ? C5 O5 1.387(8) . ? C6 H6 0.9300 . ? C7 O2 1.226(7) . ? C7 O1 1.259(7) . ? C8 O3 1.248(8) . ? C8 O4 1.251(8) . ? C9 O5 1.414(8) . ? C9 C10 1.507(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.372(11) . ? C10 C15 1.392(10) . ? C11 C12 1.396(10) . ? C11 H11 0.9300 . ? C12 C13 1.370(9) . ? C12 H12 0.9300 . ? C13 C14 1.400(10) . ? C13 C16 1.500(9) . ? C14 C15 1.357(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.382(9) . ? C16 C17 1.386(10) . ? C17 C18 1.379(11) . ? C17 H17 0.9300 . ? C18 C19 1.381(13) . ? C18 H18 0.9300 . ? C19 C20 1.367(12) . ? C19 H19 0.9300 . ? C20 C21 1.396(10) . ? C20 H20 0.9300 . ? C21 C22 1.505(10) . ? C22 O7 1.254(7) . ? C22 O6 1.273(7) . ? C23 C28 1.389(9) . ? C23 C24 1.393(8) . ? C23 C29 1.509(9) . ? C24 C25 1.362(9) . ? C24 H24 0.9300 . ? C25 C26 1.381(9) . ? C25 C30 1.513(8) . ? C26 C27 1.381(8) . ? C26 H26 0.9300 . ? C27 O12 1.365(7) . ? C27 C28 1.384(9) . ? C28 H28 0.9300 . ? C29 O10 1.263(8) . ? C29 O11 1.261(7) . ? C30 O9 1.249(8) . ? C30 O8 1.252(8) . ? C31 O12 1.403(8) . ? C31 C32 1.497(9) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C37 1.362(9) . ? C32 C33 1.390(11) . ? C33 C34 1.360(10) . ? C33 H33 0.9300 . ? C34 C35 1.407(10) . ? C34 H34 0.9300 . ? C35 C36 1.365(10) . ? C35 C38 1.485(9) . ? C36 C37 1.393(9) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.372(10) . ? C38 C43 1.409(9) . ? C39 C40 1.377(11) . ? C39 H39 0.9300 . ? C40 C41 1.348(12) . ? C40 H40 0.9300 . ? C41 C42 1.366(11) . ? C41 H41 0.9300 . ? C42 C43 1.383(9) . ? C42 H42 0.9300 . ? C43 C44 1.501(10) . ? C44 O13 1.253(8) . ? C44 O14 1.270(8) . ? O1 Zn5 1.974(4) 1_655 ? O6 Zn3 1.987(5) 1_556 ? O7 Zn2 2.088(5) 1_556 ? O10 Zn4 2.237(5) 1_655 ? O10 Zn2 2.367(5) 1_655 ? O11 Zn1 1.968(5) 1_655 ? O13 Zn2 2.140(4) 2_766 ? O14 Zn3 1.942(5) 2_766 ? O15 Zn5 2.020(4) 1_655 ? O16 Zn4 2.141(4) 2_656 ? O18 Zn4 2.052(5) 2_656 ? O19 Zn5 1.972(5) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Zn1 O17 115.4(2) . . ? O8 Zn1 O11 112.2(2) . 1_455 ? O17 Zn1 O11 108.9(2) . 1_455 ? O8 Zn1 O15 106.87(19) . . ? O17 Zn1 O15 109.2(2) . . ? O11 Zn1 O15 103.4(2) 1_455 . ? O17 Zn2 O18 169.88(18) . . ? O17 Zn2 O7 92.78(19) . 1_554 ? O18 Zn2 O7 90.22(17) . 1_554 ? O17 Zn2 O16 94.73(19) . . ? O18 Zn2 O16 80.79(17) . . ? O7 Zn2 O16 167.75(18) 1_554 . ? O17 Zn2 O13 88.88(19) . 2_766 ? O18 Zn2 O13 100.44(17) . 2_766 ? O7 Zn2 O13 95.72(19) 1_554 2_766 ? O16 Zn2 O13 94.09(18) . 2_766 ? O17 Zn2 O10 85.55(17) . 1_455 ? O18 Zn2 O10 84.74(15) . 1_455 ? O7 Zn2 O10 91.10(17) 1_554 1_455 ? O16 Zn2 O10 79.87(16) . 1_455 ? O13 Zn2 O10 171.40(17) 2_766 1_455 ? O17 Zn2 Zn3 150.78(14) . . ? O18 Zn2 Zn3 38.67(11) . . ? O7 Zn2 Zn3 68.82(11) 1_554 . ? O16 Zn2 Zn3 107.67(11) . . ? O13 Zn2 Zn3 71.42(12) 2_766 . ? O10 Zn2 Zn3 116.15(10) 1_455 . ? O19 Zn3 O14 112.2(2) . 2_766 ? O19 Zn3 O18 106.74(19) . . ? O14 Zn3 O18 117.72(19) 2_766 . ? O19 Zn3 O6 114.7(2) . 1_554 ? O14 Zn3 O6 109.9(2) 2_766 1_554 ? O18 Zn3 O6 94.68(19) . 1_554 ? O19 Zn3 Zn2 145.88(15) . . ? O14 Zn3 Zn2 83.94(14) 2_766 . ? O18 Zn3 Zn2 41.18(11) . . ? O6 Zn3 Zn2 84.91(12) 1_554 . ? O16 Zn4 O2 170.9(2) . . ? O16 Zn4 O18 96.59(18) . 2_656 ? O2 Zn4 O18 90.50(19) . 2_656 ? O16 Zn4 O16 82.44(18) . 2_656 ? O2 Zn4 O16 93.18(16) . 2_656 ? O18 Zn4 O16 80.21(16) 2_656 2_656 ? O16 Zn4 O15 94.53(16) . . ? O2 Zn4 O15 90.50(16) . . ? O18 Zn4 O15 95.23(17) 2_656 . ? O16 Zn4 O15 174.16(17) 2_656 . ? O16 Zn4 O10 84.55(18) . 1_455 ? O2 Zn4 O10 87.69(19) . 1_455 ? O18 Zn4 O10 172.52(16) 2_656 1_455 ? O16 Zn4 O10 92.64(16) 2_656 1_455 ? O15 Zn4 O10 92.04(16) . 1_455 ? O16 Zn4 Zn4 42.57(12) . 2_656 ? O2 Zn4 Zn4 132.56(12) . 2_656 ? O18 Zn4 Zn4 87.60(11) 2_656 2_656 ? O16 Zn4 Zn4 39.87(11) 2_656 2_656 ? O15 Zn4 Zn4 136.88(12) . 2_656 ? O10 Zn4 Zn4 88.28(11) 1_455 2_656 ? O19 Zn5 O1 104.5(2) 2_556 1_455 ? O19 Zn5 O4 106.67(19) 2_556 . ? O1 Zn5 O4 107.92(19) 1_455 . ? O19 Zn5 O15 111.42(19) 2_556 1_455 ? O1 Zn5 O15 103.72(18) 1_455 1_455 ? O4 Zn5 O15 121.31(19) . 1_455 ? C6 C1 C2 118.7(6) . . ? C6 C1 C7 120.8(5) . . ? C2 C1 C7 120.5(5) . . ? C3 C2 C1 120.9(6) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 C8 120.0(6) . . ? C4 C3 C8 120.6(6) . . ? C5 C4 C3 119.3(6) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 120.8(6) . . ? C6 C5 O5 123.4(5) . . ? C4 C5 O5 115.8(6) . . ? C5 C6 C1 120.7(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? O2 C7 O1 125.1(6) . . ? O2 C7 C1 116.7(5) . . ? O1 C7 C1 118.2(5) . . ? O3 C8 O4 122.0(6) . . ? O3 C8 C3 119.4(6) . . ? O4 C8 C3 118.6(6) . . ? O5 C9 C10 110.0(6) . . ? O5 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? O5 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C15 119.4(6) . . ? C11 C10 C9 125.4(6) . . ? C15 C10 C9 115.2(7) . . ? C10 C11 C12 119.9(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 121.6(7) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 117.0(6) . . ? C12 C13 C16 123.1(7) . . ? C14 C13 C16 119.9(6) . . ? C15 C14 C13 122.3(7) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C10 119.8(7) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C21 C16 C17 119.3(6) . . ? C21 C16 C13 121.7(6) . . ? C17 C16 C13 118.6(6) . . ? C18 C17 C16 121.3(7) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 119.2(8) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 119.9(8) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.2(8) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 119.0(7) . . ? C16 C21 C22 122.9(6) . . ? C20 C21 C22 117.9(6) . . ? O7 C22 O6 124.4(7) . . ? O7 C22 C21 118.8(6) . . ? O6 C22 C21 116.8(5) . . ? C28 C23 C24 119.1(6) . . ? C28 C23 C29 120.7(5) . . ? C24 C23 C29 119.9(6) . . ? C25 C24 C23 120.3(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.4(5) . . ? C24 C25 C30 121.2(6) . . ? C26 C25 C30 118.3(6) . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? O12 C27 C26 124.0(6) . . ? O12 C27 C28 116.7(5) . . ? C26 C27 C28 119.2(6) . . ? C27 C28 C23 120.5(5) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? O10 C29 O11 124.5(6) . . ? O10 C29 C23 118.7(5) . . ? O11 C29 C23 116.7(6) . . ? O9 C30 O8 124.2(6) . . ? O9 C30 C25 119.3(6) . . ? O8 C30 C25 116.5(6) . . ? O12 C31 C32 110.0(5) . . ? O12 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O12 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C37 C32 C33 117.7(7) . . ? C37 C32 C31 123.2(7) . . ? C33 C32 C31 119.2(6) . . ? C34 C33 C32 121.4(7) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C35 121.3(7) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 116.4(7) . . ? C36 C35 C38 123.0(6) . . ? C34 C35 C38 120.5(7) . . ? C35 C36 C37 122.0(6) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C32 C37 C36 120.9(7) . . ? C32 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C39 C38 C43 117.5(7) . . ? C39 C38 C35 119.9(6) . . ? C43 C38 C35 122.6(6) . . ? C38 C39 C40 122.1(8) . . ? C38 C39 H39 118.9 . . ? C40 C39 H39 118.9 . . ? C41 C40 C39 120.0(8) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 119.8(8) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C43 121.2(7) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C42 C43 C38 119.1(6) . . ? C42 C43 C44 117.9(6) . . ? C38 C43 C44 123.0(6) . . ? O13 C44 O14 124.8(6) . . ? O13 C44 C43 119.5(6) . . ? O14 C44 C43 115.6(6) . . ? C7 O1 Zn5 119.4(4) . 1_655 ? C7 O2 Zn4 143.6(4) . . ? C8 O4 Zn5 106.3(4) . . ? C5 O5 C9 115.5(5) . . ? C22 O6 Zn3 119.0(4) . 1_556 ? C22 O7 Zn2 136.7(4) . 1_556 ? C30 O8 Zn1 112.9(4) . . ? C29 O10 Zn4 122.0(4) . 1_655 ? C29 O10 Zn2 130.8(4) . 1_655 ? Zn4 O10 Zn2 90.37(16) 1_655 1_655 ? C29 O11 Zn1 112.0(4) . 1_655 ? C27 O12 C31 116.9(5) . . ? C44 O13 Zn2 131.8(5) . 2_766 ? C44 O14 Zn3 125.1(4) . 2_766 ? Zn1 O15 Zn5 119.5(2) . 1_655 ? Zn1 O15 Zn4 105.17(19) . . ? Zn5 O15 Zn4 110.02(19) 1_655 . ? Zn4 O16 Zn2 104.70(19) . . ? Zn4 O16 Zn4 97.56(18) . 2_656 ? Zn2 O16 Zn4 97.10(17) . 2_656 ? Zn1 O17 Zn2 117.7(2) . . ? Zn3 O18 Zn4 122.2(2) . 2_656 ? Zn3 O18 Zn2 100.15(18) . . ? Zn4 O18 Zn2 100.81(18) 2_656 . ? Zn3 O19 Zn5 119.5(2) . 2_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O17 Zn2 Zn3 O19 161.6(4) . . . . ? O18 Zn2 Zn3 O19 -24.9(3) . . . . ? O7 Zn2 Zn3 O19 -144.3(3) 1_554 . . . ? O16 Zn2 Zn3 O19 23.3(3) . . . . ? O13 Zn2 Zn3 O19 111.7(3) 2_766 . . . ? O10 Zn2 Zn3 O19 -63.9(3) 1_455 . . . ? O17 Zn2 Zn3 O14 40.2(4) . . . 2_766 ? O18 Zn2 Zn3 O14 -146.3(3) . . . 2_766 ? O7 Zn2 Zn3 O14 94.3(2) 1_554 . . 2_766 ? O16 Zn2 Zn3 O14 -98.1(2) . . . 2_766 ? O13 Zn2 Zn3 O14 -9.7(2) 2_766 . . 2_766 ? O10 Zn2 Zn3 O14 174.7(2) 1_455 . . 2_766 ? O17 Zn2 Zn3 O18 -173.5(4) . . . . ? O7 Zn2 Zn3 O18 -119.4(2) 1_554 . . . ? O16 Zn2 Zn3 O18 48.2(2) . . . . ? O13 Zn2 Zn3 O18 136.6(2) 2_766 . . . ? O10 Zn2 Zn3 O18 -39.0(2) 1_455 . . . ? O17 Zn2 Zn3 O6 -70.4(4) . . . 1_554 ? O18 Zn2 Zn3 O6 103.1(2) . . . 1_554 ? O7 Zn2 Zn3 O6 -16.3(2) 1_554 . . 1_554 ? O16 Zn2 Zn3 O6 151.24(19) . . . 1_554 ? O13 Zn2 Zn3 O6 -120.4(2) 2_766 . . 1_554 ? O10 Zn2 Zn3 O6 64.07(19) 1_455 . . 1_554 ? C6 C1 C2 C3 -0.5(10) . . . . ? C7 C1 C2 C3 179.0(6) . . . . ? C1 C2 C3 C4 0.8(10) . . . . ? C1 C2 C3 C8 179.5(6) . . . . ? C2 C3 C4 C5 -1.7(10) . . . . ? C8 C3 C4 C5 179.6(7) . . . . ? C3 C4 C5 C6 2.3(11) . . . . ? C3 C4 C5 O5 -178.7(6) . . . . ? C4 C5 C6 C1 -2.1(11) . . . . ? O5 C5 C6 C1 179.1(7) . . . . ? C2 C1 C6 C5 1.1(10) . . . . ? C7 C1 C6 C5 -178.4(7) . . . . ? C6 C1 C7 O2 -178.9(6) . . . . ? C2 C1 C7 O2 1.6(10) . . . . ? C6 C1 C7 O1 1.3(10) . . . . ? C2 C1 C7 O1 -178.3(6) . . . . ? C2 C3 C8 O3 2.9(10) . . . . ? C4 C3 C8 O3 -178.4(7) . . . . ? C2 C3 C8 O4 -177.5(7) . . . . ? C4 C3 C8 O4 1.2(10) . . . . ? O5 C9 C10 C11 -28.0(11) . . . . ? O5 C9 C10 C15 153.6(7) . . . . ? C15 C10 C11 C12 1.6(11) . . . . ? C9 C10 C11 C12 -176.7(7) . . . . ? C10 C11 C12 C13 -3.1(11) . . . . ? C11 C12 C13 C14 4.0(11) . . . . ? C11 C12 C13 C16 -177.5(6) . . . . ? C12 C13 C14 C15 -3.7(11) . . . . ? C16 C13 C14 C15 177.7(7) . . . . ? C13 C14 C15 C10 2.4(12) . . . . ? C11 C10 C15 C14 -1.3(12) . . . . ? C9 C10 C15 C14 177.2(7) . . . . ? C12 C13 C16 C21 136.2(7) . . . . ? C14 C13 C16 C21 -45.3(9) . . . . ? C12 C13 C16 C17 -50.8(9) . . . . ? C14 C13 C16 C17 127.7(8) . . . . ? C21 C16 C17 C18 -2.1(12) . . . . ? C13 C16 C17 C18 -175.3(7) . . . . ? C16 C17 C18 C19 -0.8(14) . . . . ? C17 C18 C19 C20 3.9(15) . . . . ? C18 C19 C20 C21 -4.1(15) . . . . ? C17 C16 C21 C20 1.9(11) . . . . ? C13 C16 C21 C20 174.9(7) . . . . ? C17 C16 C21 C22 176.7(6) . . . . ? C13 C16 C21 C22 -10.4(10) . . . . ? C19 C20 C21 C16 1.1(12) . . . . ? C19 C20 C21 C22 -173.8(8) . . . . ? C16 C21 C22 O7 139.9(7) . . . . ? C20 C21 C22 O7 -45.3(9) . . . . ? C16 C21 C22 O6 -39.0(10) . . . . ? C20 C21 C22 O6 135.8(7) . . . . ? C28 C23 C24 C25 0.9(10) . . . . ? C29 C23 C24 C25 175.0(6) . . . . ? C23 C24 C25 C26 -0.3(10) . . . . ? C23 C24 C25 C30 -178.3(6) . . . . ? C24 C25 C26 C27 -1.1(10) . . . . ? C30 C25 C26 C27 177.0(7) . . . . ? C25 C26 C27 O12 -177.9(7) . . . . ? C25 C26 C27 C28 1.8(11) . . . . ? O12 C27 C28 C23 178.6(6) . . . . ? C26 C27 C28 C23 -1.1(11) . . . . ? C24 C23 C28 C27 -0.2(10) . . . . ? C29 C23 C28 C27 -174.2(7) . . . . ? C28 C23 C29 O10 165.9(6) . . . . ? C24 C23 C29 O10 -8.0(10) . . . . ? C28 C23 C29 O11 -11.6(10) . . . . ? C24 C23 C29 O11 174.4(6) . . . . ? C24 C25 C30 O9 4.1(11) . . . . ? C26 C25 C30 O9 -173.9(7) . . . . ? C24 C25 C30 O8 -176.9(7) . . . . ? C26 C25 C30 O8 5.0(10) . . . . ? O12 C31 C32 C37 -23.9(10) . . . . ? O12 C31 C32 C33 157.8(7) . . . . ? C37 C32 C33 C34 0.7(13) . . . . ? C31 C32 C33 C34 179.1(8) . . . . ? C32 C33 C34 C35 4.6(15) . . . . ? C33 C34 C35 C36 -6.8(13) . . . . ? C33 C34 C35 C38 175.3(8) . . . . ? C34 C35 C36 C37 4.1(11) . . . . ? C38 C35 C36 C37 -178.1(7) . . . . ? C33 C32 C37 C36 -3.5(11) . . . . ? C31 C32 C37 C36 178.2(7) . . . . ? C35 C36 C37 C32 1.0(11) . . . . ? C36 C35 C38 C39 -137.8(9) . . . . ? C34 C35 C38 C39 39.9(12) . . . . ? C36 C35 C38 C43 42.9(11) . . . . ? C34 C35 C38 C43 -139.4(8) . . . . ? C43 C38 C39 C40 -1.6(14) . . . . ? C35 C38 C39 C40 179.0(9) . . . . ? C38 C39 C40 C41 0.3(16) . . . . ? C39 C40 C41 C42 -1.6(16) . . . . ? C40 C41 C42 C43 4.3(15) . . . . ? C41 C42 C43 C38 -5.6(12) . . . . ? C41 C42 C43 C44 175.9(8) . . . . ? C39 C38 C43 C42 4.2(12) . . . . ? C35 C38 C43 C42 -176.5(7) . . . . ? C39 C38 C43 C44 -177.4(8) . . . . ? C35 C38 C43 C44 1.9(12) . . . . ? C42 C43 C44 O13 -133.9(7) . . . . ? C38 C43 C44 O13 47.7(11) . . . . ? C42 C43 C44 O14 44.4(10) . . . . ? C38 C43 C44 O14 -134.0(7) . . . . ? O2 C7 O1 Zn5 -7.7(9) . . . 1_655 ? C1 C7 O1 Zn5 172.1(4) . . . 1_655 ? O1 C7 O2 Zn4 -34.6(12) . . . . ? C1 C7 O2 Zn4 145.6(6) . . . . ? O16 Zn4 O2 C7 -104.4(12) . . . . ? O18 Zn4 O2 C7 114.4(8) 2_656 . . . ? O16 Zn4 O2 C7 -165.3(8) 2_656 . . . ? O15 Zn4 O2 C7 19.2(8) . . . . ? O10 Zn4 O2 C7 -72.8(8) 1_455 . . . ? Zn4 Zn4 O2 C7 -158.3(7) 2_656 . . . ? O3 C8 O4 Zn5 2.9(9) . . . . ? C3 C8 O4 Zn5 -176.7(5) . . . . ? O19 Zn5 O4 C8 74.2(5) 2_556 . . . ? O1 Zn5 O4 C8 -174.0(5) 1_455 . . . ? O15 Zn5 O4 C8 -54.8(5) 1_455 . . . ? C6 C5 O5 C9 2.2(11) . . . . ? C4 C5 O5 C9 -176.7(7) . . . . ? C10 C9 O5 C5 -175.8(7) . . . . ? O7 C22 O6 Zn3 -14.2(9) . . . 1_556 ? C21 C22 O6 Zn3 164.6(4) . . . 1_556 ? O6 C22 O7 Zn2 -13.9(11) . . . 1_556 ? C21 C22 O7 Zn2 167.3(4) . . . 1_556 ? O9 C30 O8 Zn1 3.9(10) . . . . ? C25 C30 O8 Zn1 -175.0(5) . . . . ? O17 Zn1 O8 C30 -52.3(6) . . . . ? O11 Zn1 O8 C30 -178.0(5) 1_455 . . . ? O15 Zn1 O8 C30 69.3(5) . . . . ? O11 C29 O10 Zn4 64.1(8) . . . 1_655 ? C23 C29 O10 Zn4 -113.2(6) . . . 1_655 ? O11 C29 O10 Zn2 -59.1(9) . . . 1_655 ? C23 C29 O10 Zn2 123.5(5) . . . 1_655 ? O10 C29 O11 Zn1 2.7(8) . . . 1_655 ? C23 C29 O11 Zn1 -179.8(4) . . . 1_655 ? C26 C27 O12 C31 11.9(10) . . . . ? C28 C27 O12 C31 -167.8(7) . . . . ? C32 C31 O12 C27 177.5(6) . . . . ? O14 C44 O13 Zn2 19.5(11) . . . 2_766 ? C43 C44 O13 Zn2 -162.4(5) . . . 2_766 ? O13 C44 O14 Zn3 -2.0(10) . . . 2_766 ? C43 C44 O14 Zn3 179.8(4) . . . 2_766 ? O8 Zn1 O15 Zn5 52.4(3) . . . 1_655 ? O17 Zn1 O15 Zn5 177.9(2) . . . 1_655 ? O11 Zn1 O15 Zn5 -66.2(2) 1_455 . . 1_655 ? O8 Zn1 O15 Zn4 176.54(19) . . . . ? O17 Zn1 O15 Zn4 -58.0(2) . . . . ? O11 Zn1 O15 Zn4 57.9(2) 1_455 . . . ? O16 Zn4 O15 Zn1 70.4(2) . . . . ? O2 Zn4 O15 Zn1 -102.0(2) . . . . ? O18 Zn4 O15 Zn1 167.49(18) 2_656 . . . ? O16 Zn4 O15 Zn1 129.0(15) 2_656 . . . ? O10 Zn4 O15 Zn1 -14.3(2) 1_455 . . . ? Zn4 Zn4 O15 Zn1 75.4(2) 2_656 . . . ? O16 Zn4 O15 Zn5 -159.7(2) . . . 1_655 ? O2 Zn4 O15 Zn5 28.0(2) . . . 1_655 ? O18 Zn4 O15 Zn5 -62.6(2) 2_656 . . 1_655 ? O16 Zn4 O15 Zn5 -101.1(16) 2_656 . . 1_655 ? O10 Zn4 O15 Zn5 115.7(2) 1_455 . . 1_655 ? Zn4 Zn4 O15 Zn5 -154.68(10) 2_656 . . 1_655 ? O2 Zn4 O16 Zn2 37.7(12) . . . . ? O18 Zn4 O16 Zn2 178.58(17) 2_656 . . . ? O16 Zn4 O16 Zn2 99.4(2) 2_656 . . . ? O15 Zn4 O16 Zn2 -85.61(19) . . . . ? O10 Zn4 O16 Zn2 6.01(17) 1_455 . . . ? Zn4 Zn4 O16 Zn2 99.4(2) 2_656 . . . ? O2 Zn4 O16 Zn4 -61.7(11) . . . 2_656 ? O18 Zn4 O16 Zn4 79.16(18) 2_656 . . 2_656 ? O16 Zn4 O16 Zn4 0.0 2_656 . . 2_656 ? O15 Zn4 O16 Zn4 174.98(18) . . . 2_656 ? O10 Zn4 O16 Zn4 -93.41(18) 1_455 . . 2_656 ? O17 Zn2 O16 Zn4 78.9(2) . . . . ? O18 Zn2 O16 Zn4 -91.99(19) . . . . ? O7 Zn2 O16 Zn4 -48.8(8) 1_554 . . . ? O13 Zn2 O16 Zn4 168.08(19) 2_766 . . . ? O10 Zn2 O16 Zn4 -5.74(16) 1_455 . . . ? Zn3 Zn2 O16 Zn4 -120.13(13) . . . . ? O17 Zn2 O16 Zn4 178.63(19) . . . 2_656 ? O18 Zn2 O16 Zn4 7.77(16) . . . 2_656 ? O7 Zn2 O16 Zn4 51.0(8) 1_554 . . 2_656 ? O13 Zn2 O16 Zn4 -92.15(17) 2_766 . . 2_656 ? O10 Zn2 O16 Zn4 94.02(17) 1_455 . . 2_656 ? Zn3 Zn2 O16 Zn4 -20.37(17) . . . 2_656 ? O8 Zn1 O17 Zn2 179.1(3) . . . . ? O11 Zn1 O17 Zn2 -53.6(3) 1_455 . . . ? O15 Zn1 O17 Zn2 58.7(3) . . . . ? O18 Zn2 O17 Zn1 0.2(14) . . . . ? O7 Zn2 O17 Zn1 107.3(3) 1_554 . . . ? O16 Zn2 O17 Zn1 -63.0(3) . . . . ? O13 Zn2 O17 Zn1 -157.0(3) 2_766 . . . ? O10 Zn2 O17 Zn1 16.4(3) 1_455 . . . ? Zn3 Zn2 O17 Zn1 156.48(12) . . . . ? O19 Zn3 O18 Zn4 56.0(3) . . . 2_656 ? O14 Zn3 O18 Zn4 -71.2(3) 2_766 . . 2_656 ? O6 Zn3 O18 Zn4 173.5(2) 1_554 . . 2_656 ? Zn2 Zn3 O18 Zn4 -109.7(3) . . . 2_656 ? O19 Zn3 O18 Zn2 165.73(19) . . . . ? O14 Zn3 O18 Zn2 38.6(3) 2_766 . . . ? O6 Zn3 O18 Zn2 -76.8(2) 1_554 . . . ? O17 Zn2 O18 Zn3 161.7(11) . . . . ? O7 Zn2 O18 Zn3 54.3(2) 1_554 . . . ? O16 Zn2 O18 Zn3 -134.0(2) . . . . ? O13 Zn2 O18 Zn3 -41.5(2) 2_766 . . . ? O10 Zn2 O18 Zn3 145.4(2) 1_455 . . . ? O17 Zn2 O18 Zn4 -72.5(12) . . . 2_656 ? O7 Zn2 O18 Zn4 -179.84(19) 1_554 . . 2_656 ? O16 Zn2 O18 Zn4 -8.20(16) . . . 2_656 ? O13 Zn2 O18 Zn4 84.3(2) 2_766 . . 2_656 ? O10 Zn2 O18 Zn4 -88.75(18) 1_455 . . 2_656 ? Zn3 Zn2 O18 Zn4 125.8(3) . . . 2_656 ? O14 Zn3 O19 Zn5 90.6(3) 2_766 . . 2_556 ? O18 Zn3 O19 Zn5 -39.7(3) . . . 2_556 ? O6 Zn3 O19 Zn5 -143.2(3) 1_554 . . 2_556 ? Zn2 Zn3 O19 Zn5 -22.9(5) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.463 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.110 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 87 43 ' ' 2 0.500 0.000 0.000 126 27 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 938333' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H43.50 N O15.25 Zn3' _chemical_formula_sum 'C50 H43.50 N O15.25 Zn3' _chemical_formula_weight 1098.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1370(7) _cell_length_b 15.3527(7) _cell_length_c 24.3497(11) _cell_angle_alpha 90 _cell_angle_beta 105.103(5) _cell_angle_gamma 90 _cell_volume 4741.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2531 _cell_measurement_theta_min 2.9594 _cell_measurement_theta_max 29.1501 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2250 _exptl_absorpt_coefficient_mu 1.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6322 _exptl_absorpt_correction_T_max 0.6754 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21971 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.1058 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8341 _reflns_number_gt 5291 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distance of O1W---H1A was restrained to 0.87+-0.02 \%A. The distance of O15...H15o was restrained to 0.87+-0.02 \%A. For C46', C47'and O1W, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8341 _refine_ls_number_parameters 655 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.04532(5) 0.21272(4) 0.35398(2) 0.02775(17) Uani 1 1 d . . . Zn2 Zn 0.00522(5) 0.34021(4) 0.25470(2) 0.02925(17) Uani 1 1 d . . . Zn3 Zn 0.09453(5) 0.13817(4) 0.23398(2) 0.03186(18) Uani 1 1 d . . . C1 C -0.2387(4) 0.3371(3) 0.35305(19) 0.0287(12) Uani 1 1 d . . . C2 C -0.2885(4) 0.4094(4) 0.3250(2) 0.0348(13) Uani 1 1 d . . . H2 H -0.2571 0.4398 0.3008 0.042 Uiso 1 1 calc R . . C3 C -0.3843(4) 0.4382(4) 0.3320(2) 0.0344(13) Uani 1 1 d . . . C4 C -0.4314(4) 0.3923(3) 0.36734(19) 0.0325(13) Uani 1 1 d . . . H4 H -0.4963 0.4101 0.3720 0.039 Uiso 1 1 calc R . . C5 C -0.3816(4) 0.3188(3) 0.3962(2) 0.0319(13) Uani 1 1 d . . . C6 C -0.2842(4) 0.2919(3) 0.38965(19) 0.0332(13) Uani 1 1 d . . . H6 H -0.2502 0.2440 0.4097 0.040 Uiso 1 1 calc R . . C7 C -0.1369(4) 0.3076(3) 0.3419(2) 0.0319(13) Uani 1 1 d . . . C8 C -0.4358(5) 0.5183(4) 0.3006(2) 0.0407(15) Uani 1 1 d . . . C9 C -0.3940(5) 0.2032(4) 0.4610(2) 0.0473(16) Uani 1 1 d . . . H9A H -0.3298 0.2185 0.4894 0.057 Uiso 1 1 calc R . . H9B H -0.3771 0.1596 0.4360 0.057 Uiso 1 1 calc R . . C10 C -0.4737(4) 0.1678(4) 0.4895(2) 0.0382(14) Uani 1 1 d . . . C11 C -0.5802(5) 0.1795(5) 0.4669(2) 0.0552(19) Uani 1 1 d . . . H11 H -0.6035 0.2129 0.4342 0.066 Uiso 1 1 calc R . . C12 C -0.6533(5) 0.1429(4) 0.4918(2) 0.0526(18) Uani 1 1 d . . . H12 H -0.7248 0.1521 0.4756 0.063 Uiso 1 1 calc R . . C13 C -0.6213(4) 0.0927(4) 0.54048(19) 0.0376(14) Uani 1 1 d . . . C14 C -0.5141(5) 0.0811(4) 0.5635(2) 0.0410(15) Uani 1 1 d . . . H14 H -0.4904 0.0482 0.5965 0.049 Uiso 1 1 calc R . . C15 C -0.4418(4) 0.1183(4) 0.5380(2) 0.0399(15) Uani 1 1 d . . . H15 H -0.3701 0.1095 0.5540 0.048 Uiso 1 1 calc R . . C16 C -0.7013(4) 0.0498(4) 0.5646(2) 0.0376(14) Uani 1 1 d . . . C17 C -0.7839(5) 0.0063(5) 0.5277(2) 0.063(2) Uani 1 1 d . . . H17 H -0.7876 0.0058 0.4891 0.076 Uiso 1 1 calc R . . C18 C -0.8606(6) -0.0360(5) 0.5466(3) 0.077(2) Uani 1 1 d . . . H18 H -0.9158 -0.0634 0.5206 0.092 Uiso 1 1 calc R . . C19 C -0.8559(5) -0.0380(5) 0.6033(3) 0.0623(19) Uani 1 1 d . . . H19 H -0.9077 -0.0670 0.6159 0.075 Uiso 1 1 calc R . . C20 C -0.7752(5) 0.0025(4) 0.6411(2) 0.0472(16) Uani 1 1 d . . . H20 H -0.7716 0.0002 0.6797 0.057 Uiso 1 1 calc R . . C21 C -0.6980(4) 0.0475(3) 0.62273(19) 0.0318(13) Uani 1 1 d . . . C22 C -0.6204(4) 0.0963(4) 0.6669(2) 0.0342(14) Uani 1 1 d . . . C23 C 0.1617(4) -0.0395(3) 0.35266(18) 0.0247(12) Uani 1 1 d . . . C24 C 0.1059(4) -0.0877(3) 0.38371(19) 0.0318(13) Uani 1 1 d . . . H24 H 0.0590 -0.0597 0.4005 0.038 Uiso 1 1 calc R . . C25 C 0.1197(4) -0.1757(3) 0.3896(2) 0.0340(13) Uani 1 1 d . . . C26 C 0.1914(4) -0.2188(3) 0.36527(19) 0.0295(12) Uani 1 1 d . . . H26 H 0.2023 -0.2785 0.3703 0.035 Uiso 1 1 calc R . . C27 C 0.2457(4) -0.1715(3) 0.33363(18) 0.0273(12) Uani 1 1 d . . . C28 C 0.2310(4) -0.0820(3) 0.32757(18) 0.0295(13) Uani 1 1 d . . . H28 H 0.2679 -0.0503 0.3065 0.035 Uiso 1 1 calc R . . C29 C 0.1444(4) 0.0558(3) 0.34513(19) 0.0291(12) Uani 1 1 d . . . C30 C 0.3188(4) -0.2157(4) 0.30473(19) 0.0300(12) Uani 1 1 d . . . C31 C -0.0235(5) -0.1931(4) 0.4319(2) 0.0491(17) Uani 1 1 d . . . H31A H -0.0718 -0.1677 0.3987 0.059 Uiso 1 1 calc R . . H31B H -0.0003 -0.1473 0.4599 0.059 Uiso 1 1 calc R . . C32 C -0.0784(5) -0.2624(4) 0.4560(2) 0.0364(14) Uani 1 1 d . . . C33 C -0.1855(5) -0.2701(4) 0.4377(2) 0.0524(18) Uani 1 1 d . . . H33 H -0.2231 -0.2359 0.4077 0.063 Uiso 1 1 calc R . . C34 C -0.2377(5) -0.3283(4) 0.4634(2) 0.0510(17) Uani 1 1 d . . . H34 H -0.3109 -0.3316 0.4512 0.061 Uiso 1 1 calc R . . C35 C -0.1846(5) -0.3821(4) 0.5071(2) 0.0360(14) Uani 1 1 d . . . C36 C -0.0761(5) -0.3768(4) 0.5230(2) 0.0504(17) Uani 1 1 d . . . H36 H -0.0378 -0.4139 0.5510 0.060 Uiso 1 1 calc R . . C37 C -0.0231(5) -0.3170(4) 0.4977(2) 0.0501(17) Uani 1 1 d . . . H37 H 0.0502 -0.3140 0.5091 0.060 Uiso 1 1 calc R . . C38 C -0.2438(4) -0.4403(4) 0.5366(2) 0.0341(13) Uani 1 1 d . . . C39 C -0.3131(5) -0.5003(4) 0.5051(2) 0.0517(18) Uani 1 1 d . . . H39 H -0.3213 -0.5033 0.4660 0.062 Uiso 1 1 calc R . . C40 C -0.3702(5) -0.5557(4) 0.5297(2) 0.0542(18) Uani 1 1 d . . . H40 H -0.4166 -0.5954 0.5075 0.065 Uiso 1 1 calc R . . C41 C -0.3586(5) -0.5523(4) 0.5873(2) 0.0513(17) Uani 1 1 d . . . H41 H -0.3976 -0.5892 0.6043 0.062 Uiso 1 1 calc R . . C42 C -0.2891(4) -0.4941(4) 0.6195(2) 0.0386(14) Uani 1 1 d . . . H42 H -0.2802 -0.4931 0.6587 0.046 Uiso 1 1 calc R . . C43 C -0.2319(4) -0.4368(3) 0.59547(19) 0.0292(12) Uani 1 1 d . . . C44 C -0.1597(4) -0.3738(4) 0.6336(2) 0.0294(12) Uani 1 1 d . . . C45 C -0.3365(7) 0.1505(6) 0.2471(3) 0.087(3) Uani 1 1 d . . . C46 C -0.3291(11) 0.2330(8) 0.2144(5) 0.052(3) Uani 0.60 1 d P . . C46' C -0.369(2) 0.2530(19) 0.2232(12) 0.090(10) Uani 0.40 1 d PU . . C47 C -0.4899(11) 0.1678(8) 0.2828(6) 0.077(4) Uani 0.60 1 d P . . C47' C -0.566(3) 0.136(2) 0.2528(13) 0.134(10) Uani 0.40 1 d PU . . C48 C -0.5726(9) 0.1265(8) 0.3014(5) 0.140(5) Uani 1 1 d . . . C49 C -0.5049(6) 0.1019(5) 0.1810(4) 0.084(3) Uani 1 1 d . . . H49A H -0.5701 0.0709 0.1793 0.101 Uiso 1 1 calc R . . H49B H -0.5236 0.1596 0.1654 0.101 Uiso 1 1 calc R . . C50 C -0.4483(8) 0.0562(5) 0.1449(3) 0.099(3) Uani 1 1 d . . . H50A H -0.4922 0.0531 0.1067 0.149 Uiso 1 1 calc R . . H50B H -0.4310 -0.0016 0.1593 0.149 Uiso 1 1 calc R . . H50C H -0.3848 0.0873 0.1452 0.149 Uiso 1 1 calc R . . N1 N -0.4449(5) 0.1108(4) 0.2419(2) 0.0668(17) Uani 1 1 d . . . O1 O -0.0889(3) 0.2447(2) 0.36996(13) 0.0343(9) Uani 1 1 d . . . O2 O -0.1085(3) 0.3475(2) 0.30377(16) 0.0479(11) Uani 1 1 d . . . O3 O -0.3869(4) 0.5607(3) 0.27241(19) 0.0715(15) Uani 1 1 d . . . O4 O -0.5262(3) 0.5378(2) 0.30619(15) 0.0448(10) Uani 1 1 d . . . O5 O -0.4371(3) 0.2784(3) 0.42914(15) 0.0449(10) Uani 1 1 d . . . O6 O -0.5661(3) 0.0540(3) 0.71017(13) 0.0420(10) Uani 1 1 d . . . O7 O -0.6118(3) 0.1759(3) 0.66530(15) 0.0510(11) Uani 1 1 d . . . O8 O 0.0925(3) 0.0935(2) 0.37517(13) 0.0319(9) Uani 1 1 d . . . O9 O 0.1823(3) 0.0938(2) 0.30892(14) 0.0359(9) Uani 1 1 d . . . O10 O 0.3762(3) -0.1679(3) 0.28474(17) 0.0547(12) Uani 1 1 d . . . O11 O 0.3166(3) -0.2976(2) 0.30302(14) 0.0387(10) Uani 1 1 d . . . O12 O 0.0643(3) -0.2292(2) 0.41665(16) 0.0476(11) Uani 1 1 d . . . O13 O -0.1090(3) -0.4012(2) 0.68092(14) 0.0420(10) Uani 1 1 d . . . O14 O -0.1564(3) -0.2959(2) 0.61661(13) 0.0362(9) Uani 1 1 d . . . O15 O 0.0046(3) 0.2100(2) 0.26900(13) 0.0271(8) Uani 1 1 d D . . H15O H -0.050(3) 0.181(3) 0.2558(19) 0.041 Uiso 1 1 d D . . O1W O -0.527(3) -0.688(2) 0.6342(13) 0.150(10) Uani 0.25 1 d PDU . . H1A H -0.54(2) -0.645(10) 0.653(9) 0.225 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0285(4) 0.0212(3) 0.0361(3) 0.0020(3) 0.0131(3) 0.0031(3) Zn2 0.0311(4) 0.0262(3) 0.0340(3) 0.0026(3) 0.0148(3) 0.0035(3) Zn3 0.0380(4) 0.0229(3) 0.0413(3) -0.0032(3) 0.0221(3) -0.0040(3) C1 0.031(3) 0.027(3) 0.031(3) 0.003(2) 0.013(2) 0.008(3) C2 0.035(4) 0.032(3) 0.044(3) 0.005(3) 0.021(3) 0.005(3) C3 0.035(4) 0.035(3) 0.036(3) 0.006(3) 0.014(3) 0.010(3) C4 0.027(3) 0.035(3) 0.040(3) 0.004(3) 0.017(2) 0.012(3) C5 0.033(3) 0.031(3) 0.037(3) 0.002(3) 0.019(3) 0.003(3) C6 0.034(4) 0.030(3) 0.037(3) 0.003(3) 0.011(2) 0.009(3) C7 0.028(3) 0.028(3) 0.042(3) -0.004(3) 0.014(3) 0.002(3) C8 0.042(4) 0.037(4) 0.046(3) 0.009(3) 0.018(3) 0.014(3) C9 0.041(4) 0.057(4) 0.050(3) 0.021(3) 0.025(3) 0.014(3) C10 0.033(4) 0.046(4) 0.039(3) 0.011(3) 0.014(3) 0.007(3) C11 0.045(4) 0.083(5) 0.042(3) 0.028(3) 0.019(3) 0.018(4) C12 0.032(4) 0.085(5) 0.041(3) 0.020(3) 0.011(3) 0.011(4) C13 0.033(4) 0.053(4) 0.027(3) -0.003(3) 0.008(3) -0.008(3) C14 0.049(4) 0.044(4) 0.029(3) 0.012(3) 0.010(3) -0.003(3) C15 0.028(4) 0.056(4) 0.033(3) 0.008(3) 0.004(2) 0.000(3) C16 0.038(4) 0.040(4) 0.032(3) -0.001(3) 0.007(3) -0.001(3) C17 0.052(5) 0.088(6) 0.045(3) -0.017(4) 0.007(3) -0.029(4) C18 0.053(5) 0.087(6) 0.080(5) -0.021(4) 0.000(4) -0.040(5) C19 0.042(5) 0.063(5) 0.085(5) 0.012(4) 0.021(4) -0.015(4) C20 0.041(4) 0.056(4) 0.047(3) 0.015(3) 0.014(3) -0.001(4) C21 0.027(3) 0.033(3) 0.034(3) 0.000(2) 0.006(2) -0.003(3) C22 0.031(4) 0.047(4) 0.028(3) 0.003(3) 0.014(2) -0.001(3) C23 0.026(3) 0.021(3) 0.028(2) 0.003(2) 0.010(2) 0.002(2) C24 0.045(4) 0.025(3) 0.033(3) -0.001(2) 0.023(3) 0.004(3) C25 0.042(4) 0.027(3) 0.038(3) 0.002(3) 0.020(3) -0.003(3) C26 0.035(3) 0.019(3) 0.037(3) 0.001(2) 0.015(2) 0.003(3) C27 0.030(3) 0.025(3) 0.028(2) -0.002(2) 0.009(2) 0.004(3) C28 0.029(3) 0.033(3) 0.031(3) 0.006(2) 0.015(2) 0.001(3) C29 0.023(3) 0.030(3) 0.033(3) 0.006(3) 0.006(2) 0.002(3) C30 0.028(3) 0.034(3) 0.029(3) 0.001(3) 0.010(2) 0.005(3) C31 0.064(5) 0.038(4) 0.060(4) -0.001(3) 0.045(3) -0.002(3) C32 0.042(4) 0.034(3) 0.041(3) -0.002(3) 0.026(3) -0.005(3) C33 0.064(5) 0.054(4) 0.046(3) 0.015(3) 0.028(3) 0.008(4) C34 0.046(4) 0.063(5) 0.046(3) 0.009(3) 0.016(3) 0.003(4) C35 0.042(4) 0.034(3) 0.036(3) -0.006(3) 0.017(3) -0.009(3) C36 0.054(5) 0.063(5) 0.037(3) 0.018(3) 0.016(3) 0.001(4) C37 0.040(4) 0.070(5) 0.044(3) 0.004(3) 0.018(3) -0.012(4) C38 0.037(4) 0.035(3) 0.034(3) 0.005(3) 0.014(2) -0.009(3) C39 0.071(5) 0.052(4) 0.037(3) -0.008(3) 0.022(3) -0.030(4) C40 0.061(5) 0.053(4) 0.050(4) -0.008(3) 0.015(3) -0.033(4) C41 0.058(5) 0.046(4) 0.057(4) -0.002(3) 0.027(3) -0.029(4) C42 0.047(4) 0.039(3) 0.033(3) 0.000(3) 0.016(3) -0.010(3) C43 0.032(3) 0.025(3) 0.033(3) 0.003(2) 0.014(2) 0.000(3) C44 0.024(3) 0.032(3) 0.037(3) -0.003(3) 0.014(2) -0.007(3) C45 0.085(7) 0.089(6) 0.074(5) 0.011(5) -0.002(4) -0.025(5) C46 0.062(9) 0.031(7) 0.065(7) -0.002(6) 0.019(7) -0.006(6) C46' 0.090(10) 0.090(10) 0.090(10) 0.0002(10) 0.023(3) -0.0002(10) C47 0.075(10) 0.064(9) 0.113(10) -0.034(8) 0.063(9) -0.017(8) C47' 0.134(10) 0.134(10) 0.134(10) 0.0000(10) 0.035(3) 0.0003(10) C48 0.140(11) 0.151(11) 0.167(10) 0.037(8) 0.106(9) 0.038(8) C49 0.045(5) 0.038(4) 0.150(8) 0.031(5) -0.010(5) -0.010(4) C50 0.178(10) 0.040(5) 0.068(5) 0.002(4) 0.011(5) -0.009(6) N1 0.069(5) 0.069(4) 0.071(4) 0.015(3) 0.033(3) 0.018(4) O1 0.029(2) 0.036(2) 0.0403(19) 0.0059(18) 0.0139(16) 0.0138(19) O2 0.051(3) 0.037(2) 0.072(3) 0.015(2) 0.044(2) 0.017(2) O3 0.058(3) 0.070(3) 0.105(3) 0.051(3) 0.055(3) 0.033(3) O4 0.039(3) 0.041(2) 0.062(2) 0.021(2) 0.027(2) 0.022(2) O5 0.037(2) 0.048(3) 0.058(2) 0.023(2) 0.0277(19) 0.015(2) O6 0.043(3) 0.049(3) 0.0324(19) 0.0026(19) 0.0061(17) -0.005(2) O7 0.057(3) 0.037(3) 0.050(2) -0.007(2) -0.001(2) -0.006(2) O8 0.034(2) 0.023(2) 0.0442(19) 0.0023(17) 0.0207(17) 0.0079(18) O9 0.034(2) 0.031(2) 0.049(2) 0.0142(18) 0.0225(18) 0.0036(18) O10 0.057(3) 0.040(3) 0.088(3) 0.006(2) 0.055(3) 0.005(2) O11 0.050(3) 0.026(2) 0.049(2) -0.0045(18) 0.0303(19) 0.006(2) O12 0.059(3) 0.030(2) 0.074(3) 0.009(2) 0.052(2) 0.002(2) O13 0.045(3) 0.038(2) 0.037(2) 0.0015(18) 0.0002(18) -0.003(2) O14 0.036(2) 0.029(2) 0.041(2) -0.0017(18) 0.0057(16) -0.0072(19) O15 0.028(2) 0.021(2) 0.0342(18) -0.0010(15) 0.0115(16) -0.0016(17) O1W 0.149(11) 0.149(11) 0.150(11) 0.000(2) 0.039(3) 0.000(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O14 1.931(4) 3_556 ? Zn1 O8 1.958(3) . ? Zn1 O1 1.964(3) . ? Zn1 O15 1.998(3) . ? Zn1 Zn2 3.0478(8) . ? Zn2 O13 2.020(4) 3_556 ? Zn2 O15 2.030(3) . ? Zn2 O10 2.036(3) 2 ? Zn2 O6 2.040(4) 4_665 ? Zn2 O2 2.145(3) . ? Zn2 O7 2.328(4) 4_665 ? Zn2 C22 2.530(5) 4_665 ? Zn3 O4 1.918(4) 2_445 ? Zn3 O11 1.923(3) 2 ? Zn3 O15 1.966(3) . ? Zn3 O9 2.007(3) . ? C1 C2 1.377(7) . ? C1 C6 1.382(6) . ? C1 C7 1.502(7) . ? C2 C3 1.385(7) . ? C2 H2 0.9300 . ? C3 C4 1.377(6) . ? C3 C8 1.511(7) . ? C4 C5 1.398(7) . ? C4 H4 0.9300 . ? C5 O5 1.366(6) . ? C5 C6 1.392(7) . ? C6 H6 0.9300 . ? C7 O2 1.249(6) . ? C7 O1 1.254(6) . ? C8 O3 1.241(6) . ? C8 O4 1.266(6) . ? C9 O5 1.423(6) . ? C9 C10 1.500(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.374(7) . ? C10 C11 1.375(8) . ? C11 C12 1.381(8) . ? C11 H11 0.9300 . ? C12 C13 1.385(7) . ? C12 H12 0.9300 . ? C13 C14 1.385(7) . ? C13 C16 1.485(7) . ? C14 C15 1.388(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.386(8) . ? C16 C21 1.405(6) . ? C17 C18 1.374(8) . ? C17 H17 0.9300 . ? C18 C19 1.366(8) . ? C18 H18 0.9300 . ? C19 C20 1.360(8) . ? C19 H19 0.9300 . ? C20 C21 1.393(7) . ? C20 H20 0.9300 . ? C21 C22 1.479(7) . ? C22 O7 1.228(6) . ? C22 O6 1.284(6) . ? C22 Zn2 2.530(5) 4_566 ? C23 C28 1.384(6) . ? C23 C24 1.394(6) . ? C23 C29 1.485(7) . ? C24 C25 1.366(7) . ? C24 H24 0.9300 . ? C25 O12 1.373(6) . ? C25 C26 1.402(7) . ? C26 C27 1.385(6) . ? C26 H26 0.9300 . ? C27 C28 1.390(7) . ? C27 C30 1.493(7) . ? C28 H28 0.9300 . ? C29 O9 1.262(5) . ? C29 O8 1.263(5) . ? C30 O10 1.238(6) . ? C30 O11 1.258(6) . ? C31 O12 1.415(6) . ? C31 C32 1.489(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.366(8) . ? C32 C37 1.370(8) . ? C33 C34 1.373(8) . ? C33 H33 0.9300 . ? C34 C35 1.383(8) . ? C34 H34 0.9300 . ? C35 C36 1.378(8) . ? C35 C38 1.488(7) . ? C36 C37 1.390(8) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.379(7) . ? C38 C43 1.401(6) . ? C39 C40 1.372(7) . ? C39 H39 0.9300 . ? C40 C41 1.370(7) . ? C40 H40 0.9300 . ? C41 C42 1.368(7) . ? C41 H41 0.9300 . ? C42 C43 1.383(7) . ? C42 H42 0.9300 . ? C43 C44 1.496(7) . ? C44 O13 1.245(6) . ? C44 O14 1.269(6) . ? C45 C46 1.514(13) . ? C45 N1 1.524(9) . ? C45 C46' 1.69(3) . ? C46 C46' 0.68(3) . ? C47 C47' 1.18(3) . ? C47 C48 1.429(15) . ? C47 N1 1.555(12) . ? C47' C48 1.22(3) . ? C47' N1 1.73(3) . ? C49 C50 1.468(10) . ? C49 N1 1.494(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? O4 Zn3 1.918(4) 2_455 ? O6 Zn2 2.040(4) 4_566 ? O7 Zn2 2.328(4) 4_566 ? O10 Zn2 2.036(3) 2_545 ? O11 Zn3 1.923(3) 2_545 ? O13 Zn2 2.020(4) 3_556 ? O14 Zn1 1.931(4) 3_556 ? O15 H15O 0.837(19) . ? O1W H1A 0.88(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Zn1 O8 111.35(15) 3_556 . ? O14 Zn1 O1 113.07(15) 3_556 . ? O8 Zn1 O1 114.83(14) . . ? O14 Zn1 O15 111.75(13) 3_556 . ? O8 Zn1 O15 103.55(13) . . ? O1 Zn1 O15 101.43(14) . . ? O14 Zn1 Zn2 80.04(10) 3_556 . ? O8 Zn1 Zn2 141.89(9) . . ? O1 Zn1 Zn2 91.04(10) . . ? O15 Zn1 Zn2 41.22(10) . . ? O13 Zn2 O15 110.83(14) 3_556 . ? O13 Zn2 O10 87.09(16) 3_556 2 ? O15 Zn2 O10 93.35(15) . 2 ? O13 Zn2 O6 99.62(15) 3_556 4_665 ? O15 Zn2 O6 148.59(15) . 4_665 ? O10 Zn2 O6 95.73(15) 2 4_665 ? O13 Zn2 O2 88.34(16) 3_556 . ? O15 Zn2 O2 85.48(13) . . ? O10 Zn2 O2 174.54(17) 2 . ? O6 Zn2 O2 87.97(14) 4_665 . ? O13 Zn2 O7 157.32(15) 3_556 4_665 ? O15 Zn2 O7 91.42(14) . 4_665 ? O10 Zn2 O7 87.27(16) 2 4_665 ? O6 Zn2 O7 59.17(14) 4_665 4_665 ? O2 Zn2 O7 98.08(15) . 4_665 ? O13 Zn2 C22 129.56(18) 3_556 4_665 ? O15 Zn2 C22 119.55(17) . 4_665 ? O10 Zn2 C22 92.06(17) 2 4_665 ? O6 Zn2 C22 30.28(16) 4_665 4_665 ? O2 Zn2 C22 93.15(15) . 4_665 ? O7 Zn2 C22 28.90(15) 4_665 4_665 ? O13 Zn2 Zn1 74.93(10) 3_556 . ? O15 Zn2 Zn1 40.45(9) . . ? O10 Zn2 Zn1 109.84(12) 2 . ? O6 Zn2 Zn1 153.30(9) 4_665 . ? O2 Zn2 Zn1 66.00(10) . . ? O7 Zn2 Zn1 127.53(10) 4_665 . ? C22 Zn2 Zn1 149.00(13) 4_665 . ? O4 Zn3 O11 115.72(14) 2_445 2 ? O4 Zn3 O15 114.66(15) 2_445 . ? O11 Zn3 O15 115.00(14) 2 . ? O4 Zn3 O9 105.82(16) 2_445 . ? O11 Zn3 O9 108.98(15) 2 . ? O15 Zn3 O9 93.67(13) . . ? C2 C1 C6 119.6(5) . . ? C2 C1 C7 119.0(4) . . ? C6 C1 C7 121.4(4) . . ? C1 C2 C3 121.7(5) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C4 C3 C2 118.9(5) . . ? C4 C3 C8 121.2(5) . . ? C2 C3 C8 119.8(5) . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? O5 C5 C6 125.4(5) . . ? O5 C5 C4 114.2(4) . . ? C6 C5 C4 120.4(4) . . ? C1 C6 C5 119.3(5) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O2 C7 O1 125.3(5) . . ? O2 C7 C1 116.1(5) . . ? O1 C7 C1 118.6(4) . . ? O3 C8 O4 124.8(5) . . ? O3 C8 C3 118.7(5) . . ? O4 C8 C3 116.5(5) . . ? O5 C9 C10 108.7(4) . . ? O5 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O5 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C15 C10 C11 117.9(5) . . ? C15 C10 C9 120.3(5) . . ? C11 C10 C9 121.8(5) . . ? C10 C11 C12 121.5(5) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 120.8(6) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 117.9(5) . . ? C12 C13 C16 119.9(5) . . ? C14 C13 C16 122.1(5) . . ? C13 C14 C15 120.6(5) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C10 C15 C14 121.4(5) . . ? C10 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C21 117.0(5) . . ? C17 C16 C13 118.2(5) . . ? C21 C16 C13 124.8(5) . . ? C18 C17 C16 122.0(5) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C19 C18 C17 120.2(6) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 119.7(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.9(5) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 120.1(5) . . ? C20 C21 C22 116.1(4) . . ? C16 C21 C22 123.7(5) . . ? O7 C22 O6 119.6(5) . . ? O7 C22 C21 122.1(5) . . ? O6 C22 C21 118.1(5) . . ? O7 C22 Zn2 66.4(3) . 4_566 ? O6 C22 Zn2 53.3(3) . 4_566 ? C21 C22 Zn2 169.7(4) . 4_566 ? C28 C23 C24 119.3(4) . . ? C28 C23 C29 120.4(4) . . ? C24 C23 C29 120.3(4) . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 O12 124.7(5) . . ? C24 C25 C26 120.5(4) . . ? O12 C25 C26 114.7(4) . . ? C27 C26 C25 119.2(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 C30 120.8(4) . . ? C28 C27 C30 119.2(4) . . ? C23 C28 C27 120.5(4) . . ? C23 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? O9 C29 O8 124.3(5) . . ? O9 C29 C23 117.8(4) . . ? O8 C29 C23 117.9(4) . . ? O10 C30 O11 126.2(5) . . ? O10 C30 C27 116.6(5) . . ? O11 C30 C27 117.2(4) . . ? O12 C31 C32 109.6(5) . . ? O12 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O12 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C37 119.5(5) . . ? C33 C32 C31 119.7(5) . . ? C37 C32 C31 120.8(6) . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 121.8(6) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C36 C35 C34 117.3(5) . . ? C36 C35 C38 122.1(5) . . ? C34 C35 C38 120.5(5) . . ? C35 C36 C37 121.0(5) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C32 C37 C36 120.1(6) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C43 118.5(5) . . ? C39 C38 C35 119.0(4) . . ? C43 C38 C35 122.6(5) . . ? C40 C39 C38 121.8(5) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C41 C40 C39 119.7(6) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C42 C41 C40 119.4(5) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C43 121.9(5) . . ? C41 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C42 C43 C38 118.7(5) . . ? C42 C43 C44 118.4(4) . . ? C38 C43 C44 122.9(4) . . ? O13 C44 O14 124.4(5) . . ? O13 C44 C43 117.0(5) . . ? O14 C44 C43 118.5(4) . . ? C46 C45 N1 118.6(8) . . ? C46 C45 C46' 23.8(9) . . ? N1 C45 C46' 101.5(11) . . ? C46' C46 C45 93(3) . . ? C46 C46' C45 63(3) . . ? C47' C47 C48 54.5(15) . . ? C47' C47 N1 77.1(18) . . ? C48 C47 N1 113.6(10) . . ? C47 C47' C48 73(2) . . ? C47 C47' N1 61.1(17) . . ? C48 C47' N1 115(2) . . ? C47' C48 C47 52.4(16) . . ? C50 C49 N1 114.8(6) . . ? C50 C49 H49A 108.6 . . ? N1 C49 H49A 108.6 . . ? C50 C49 H49B 108.6 . . ? N1 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 N1 C45 111.0(5) . . ? C49 N1 C47 119.8(8) . . ? C45 N1 C47 103.0(7) . . ? C49 N1 C47' 84.5(11) . . ? C45 N1 C47' 141.0(13) . . ? C47 N1 C47' 41.8(10) . . ? C7 O1 Zn1 115.8(3) . . ? C7 O2 Zn2 140.9(3) . . ? C8 O4 Zn3 117.6(3) . 2_455 ? C5 O5 C9 119.5(4) . . ? C22 O6 Zn2 96.5(3) . 4_566 ? C22 O7 Zn2 84.7(3) . 4_566 ? C29 O8 Zn1 117.2(3) . . ? C29 O9 Zn3 123.7(3) . . ? C30 O10 Zn2 147.2(4) . 2_545 ? C30 O11 Zn3 121.1(3) . 2_545 ? C25 O12 C31 117.6(4) . . ? C44 O13 Zn2 130.7(4) . 3_556 ? C44 O14 Zn1 126.1(3) . 3_556 ? Zn3 O15 Zn1 115.59(17) . . ? Zn3 O15 Zn2 116.63(15) . . ? Zn1 O15 Zn2 98.33(14) . . ? Zn3 O15 H15O 95(4) . . ? Zn1 O15 H15O 112(3) . . ? Zn2 O15 H15O 120(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O14 Zn1 Zn2 O13 -11.61(15) 3_556 . . 3_556 ? O8 Zn1 Zn2 O13 -123.6(2) . . . 3_556 ? O1 Zn1 Zn2 O13 101.65(15) . . . 3_556 ? O15 Zn1 Zn2 O13 -152.08(18) . . . 3_556 ? O14 Zn1 Zn2 O15 140.48(18) 3_556 . . . ? O8 Zn1 Zn2 O15 28.5(2) . . . . ? O1 Zn1 Zn2 O15 -106.27(18) . . . . ? O14 Zn1 Zn2 O10 69.59(17) 3_556 . . 2 ? O8 Zn1 Zn2 O10 -42.4(2) . . . 2 ? O1 Zn1 Zn2 O10 -177.16(16) . . . 2 ? O15 Zn1 Zn2 O10 -70.89(19) . . . 2 ? O14 Zn1 Zn2 O6 -93.0(3) 3_556 . . 4_665 ? O8 Zn1 Zn2 O6 155.0(3) . . . 4_665 ? O1 Zn1 Zn2 O6 20.3(3) . . . 4_665 ? O15 Zn1 Zn2 O6 126.6(3) . . . 4_665 ? O14 Zn1 Zn2 O2 -106.60(16) 3_556 . . . ? O8 Zn1 Zn2 O2 141.4(2) . . . . ? O1 Zn1 Zn2 O2 6.65(16) . . . . ? O15 Zn1 Zn2 O2 112.92(19) . . . . ? O14 Zn1 Zn2 O7 171.92(17) 3_556 . . 4_665 ? O8 Zn1 Zn2 O7 59.9(2) . . . 4_665 ? O1 Zn1 Zn2 O7 -74.83(17) . . . 4_665 ? O15 Zn1 Zn2 O7 31.44(19) . . . 4_665 ? O14 Zn1 Zn2 C22 -158.0(3) 3_556 . . 4_665 ? O8 Zn1 Zn2 C22 90.0(3) . . . 4_665 ? O1 Zn1 Zn2 C22 -44.7(3) . . . 4_665 ? O15 Zn1 Zn2 C22 61.6(3) . . . 4_665 ? C6 C1 C2 C3 -0.7(8) . . . . ? C7 C1 C2 C3 177.8(5) . . . . ? C1 C2 C3 C4 -0.9(8) . . . . ? C1 C2 C3 C8 179.7(5) . . . . ? C2 C3 C4 C5 1.1(8) . . . . ? C8 C3 C4 C5 -179.5(5) . . . . ? C3 C4 C5 O5 -179.1(4) . . . . ? C3 C4 C5 C6 0.3(8) . . . . ? C2 C1 C6 C5 2.0(8) . . . . ? C7 C1 C6 C5 -176.4(5) . . . . ? O5 C5 C6 C1 177.4(5) . . . . ? C4 C5 C6 C1 -1.8(8) . . . . ? C2 C1 C7 O2 -5.8(7) . . . . ? C6 C1 C7 O2 172.7(5) . . . . ? C2 C1 C7 O1 176.0(5) . . . . ? C6 C1 C7 O1 -5.5(8) . . . . ? C4 C3 C8 O3 175.1(5) . . . . ? C2 C3 C8 O3 -5.5(8) . . . . ? C4 C3 C8 O4 -3.6(8) . . . . ? C2 C3 C8 O4 175.8(5) . . . . ? O5 C9 C10 C15 -155.5(5) . . . . ? O5 C9 C10 C11 27.8(8) . . . . ? C15 C10 C11 C12 -0.1(9) . . . . ? C9 C10 C11 C12 176.6(6) . . . . ? C10 C11 C12 C13 -0.1(10) . . . . ? C11 C12 C13 C14 0.5(9) . . . . ? C11 C12 C13 C16 -176.5(5) . . . . ? C12 C13 C14 C15 -0.6(8) . . . . ? C16 C13 C14 C15 176.3(5) . . . . ? C11 C10 C15 C14 0.0(9) . . . . ? C9 C10 C15 C14 -176.8(5) . . . . ? C13 C14 C15 C10 0.4(9) . . . . ? C12 C13 C16 C17 45.6(8) . . . . ? C14 C13 C16 C17 -131.2(6) . . . . ? C12 C13 C16 C21 -136.3(6) . . . . ? C14 C13 C16 C21 46.8(8) . . . . ? C21 C16 C17 C18 1.1(10) . . . . ? C13 C16 C17 C18 179.2(7) . . . . ? C16 C17 C18 C19 -1.5(12) . . . . ? C17 C18 C19 C20 0.3(12) . . . . ? C18 C19 C20 C21 1.1(10) . . . . ? C19 C20 C21 C16 -1.5(9) . . . . ? C19 C20 C21 C22 174.1(6) . . . . ? C17 C16 C21 C20 0.4(8) . . . . ? C13 C16 C21 C20 -177.6(5) . . . . ? C17 C16 C21 C22 -174.8(6) . . . . ? C13 C16 C21 C22 7.1(9) . . . . ? C20 C21 C22 O7 -117.4(6) . . . . ? C16 C21 C22 O7 58.0(8) . . . . ? C20 C21 C22 O6 57.6(7) . . . . ? C16 C21 C22 O6 -127.0(5) . . . . ? C20 C21 C22 Zn2 27(3) . . . 4_566 ? C16 C21 C22 Zn2 -158(2) . . . 4_566 ? C28 C23 C24 C25 0.3(8) . . . . ? C29 C23 C24 C25 178.4(5) . . . . ? C23 C24 C25 O12 -176.3(5) . . . . ? C23 C24 C25 C26 1.0(8) . . . . ? C24 C25 C26 C27 -2.0(8) . . . . ? O12 C25 C26 C27 175.5(5) . . . . ? C25 C26 C27 C28 1.7(7) . . . . ? C25 C26 C27 C30 -177.1(5) . . . . ? C24 C23 C28 C27 -0.6(7) . . . . ? C29 C23 C28 C27 -178.7(5) . . . . ? C26 C27 C28 C23 -0.4(7) . . . . ? C30 C27 C28 C23 178.4(4) . . . . ? C28 C23 C29 O9 10.2(7) . . . . ? C24 C23 C29 O9 -168.0(4) . . . . ? C28 C23 C29 O8 -170.1(5) . . . . ? C24 C23 C29 O8 11.8(7) . . . . ? C26 C27 C30 O10 -169.3(5) . . . . ? C28 C27 C30 O10 11.9(7) . . . . ? C26 C27 C30 O11 10.6(7) . . . . ? C28 C27 C30 O11 -168.2(5) . . . . ? O12 C31 C32 C33 -132.7(5) . . . . ? O12 C31 C32 C37 49.2(7) . . . . ? C37 C32 C33 C34 4.3(8) . . . . ? C31 C32 C33 C34 -173.8(5) . . . . ? C32 C33 C34 C35 -1.9(9) . . . . ? C33 C34 C35 C36 -1.7(8) . . . . ? C33 C34 C35 C38 176.1(5) . . . . ? C34 C35 C36 C37 2.8(8) . . . . ? C38 C35 C36 C37 -174.9(5) . . . . ? C33 C32 C37 C36 -3.1(8) . . . . ? C31 C32 C37 C36 174.9(5) . . . . ? C35 C36 C37 C32 -0.5(9) . . . . ? C36 C35 C38 C39 -124.7(6) . . . . ? C34 C35 C38 C39 57.7(8) . . . . ? C36 C35 C38 C43 55.2(8) . . . . ? C34 C35 C38 C43 -122.4(6) . . . . ? C43 C38 C39 C40 0.3(10) . . . . ? C35 C38 C39 C40 -179.8(6) . . . . ? C38 C39 C40 C41 -0.2(10) . . . . ? C39 C40 C41 C42 -0.7(10) . . . . ? C40 C41 C42 C43 1.7(10) . . . . ? C41 C42 C43 C38 -1.6(8) . . . . ? C41 C42 C43 C44 178.4(6) . . . . ? C39 C38 C43 C42 0.6(8) . . . . ? C35 C38 C43 C42 -179.2(5) . . . . ? C39 C38 C43 C44 -179.4(5) . . . . ? C35 C38 C43 C44 0.7(8) . . . . ? C42 C43 C44 O13 39.4(7) . . . . ? C38 C43 C44 O13 -140.6(5) . . . . ? C42 C43 C44 O14 -138.5(5) . . . . ? C38 C43 C44 O14 41.6(7) . . . . ? N1 C45 C46 C46' 48(3) . . . . ? N1 C45 C46' C46 -138(3) . . . . ? N1 C47 C47' C48 131.9(15) . . . . ? C48 C47 C47' N1 -131.9(15) . . . . ? N1 C47' C48 C47 45.9(17) . . . . ? N1 C47 C48 C47' -52(2) . . . . ? C50 C49 N1 C45 52.4(8) . . . . ? C50 C49 N1 C47 172.2(7) . . . . ? C50 C49 N1 C47' -164.6(13) . . . . ? C46 C45 N1 C49 49.9(10) . . . . ? C46' C45 N1 C49 67.6(11) . . . . ? C46 C45 N1 C47 -79.6(10) . . . . ? C46' C45 N1 C47 -61.9(11) . . . . ? C46 C45 N1 C47' -58.2(19) . . . . ? C46' C45 N1 C47' -40(2) . . . . ? C47' C47 N1 C49 36.0(19) . . . . ? C48 C47 N1 C49 77.4(13) . . . . ? C47' C47 N1 C45 159.9(18) . . . . ? C48 C47 N1 C45 -158.8(11) . . . . ? C48 C47 N1 C47' 41.4(16) . . . . ? C47 C47' N1 C49 -149.2(17) . . . . ? C48 C47' N1 C49 159(3) . . . . ? C47 C47' N1 C45 -32(3) . . . . ? C48 C47' N1 C45 -84(3) . . . . ? C48 C47' N1 C47 -52(2) . . . . ? O2 C7 O1 Zn1 3.5(7) . . . . ? C1 C7 O1 Zn1 -178.4(3) . . . . ? O14 Zn1 O1 C7 72.1(4) 3_556 . . . ? O8 Zn1 O1 C7 -158.6(3) . . . . ? O15 Zn1 O1 C7 -47.7(4) . . . . ? Zn2 Zn1 O1 C7 -7.5(4) . . . . ? O1 C7 O2 Zn2 8.7(10) . . . . ? C1 C7 O2 Zn2 -169.4(4) . . . . ? O13 Zn2 O2 C7 -85.0(6) 3_556 . . . ? O15 Zn2 O2 C7 26.0(6) . . . . ? O10 Zn2 O2 C7 -51.9(19) 2 . . . ? O6 Zn2 O2 C7 175.3(6) 4_665 . . . ? O7 Zn2 O2 C7 116.8(6) 4_665 . . . ? C22 Zn2 O2 C7 145.5(6) 4_665 . . . ? Zn1 Zn2 O2 C7 -10.8(6) . . . . ? O3 C8 O4 Zn3 2.3(8) . . . 2_455 ? C3 C8 O4 Zn3 -179.2(4) . . . 2_455 ? C6 C5 O5 C9 1.3(8) . . . . ? C4 C5 O5 C9 -179.4(5) . . . . ? C10 C9 O5 C5 -175.6(4) . . . . ? O7 C22 O6 Zn2 1.7(5) . . . 4_566 ? C21 C22 O6 Zn2 -173.5(4) . . . 4_566 ? O6 C22 O7 Zn2 -1.5(5) . . . 4_566 ? C21 C22 O7 Zn2 173.5(4) . . . 4_566 ? O9 C29 O8 Zn1 12.2(7) . . . . ? C23 C29 O8 Zn1 -167.6(3) . . . . ? O14 Zn1 O8 C29 -81.8(4) 3_556 . . . ? O1 Zn1 O8 C29 148.1(3) . . . . ? O15 Zn1 O8 C29 38.4(4) . . . . ? Zn2 Zn1 O8 C29 19.6(4) . . . . ? O8 C29 O9 Zn3 -72.2(6) . . . . ? C23 C29 O9 Zn3 107.5(5) . . . . ? O4 Zn3 O9 C29 -61.4(4) 2_445 . . . ? O11 Zn3 O9 C29 173.5(4) 2 . . . ? O15 Zn3 O9 C29 55.5(4) . . . . ? O11 C30 O10 Zn2 -4.3(11) . . . 2_545 ? C27 C30 O10 Zn2 175.6(5) . . . 2_545 ? O10 C30 O11 Zn3 -1.0(7) . . . 2_545 ? C27 C30 O11 Zn3 179.1(3) . . . 2_545 ? C24 C25 O12 C31 10.0(8) . . . . ? C26 C25 O12 C31 -167.5(5) . . . . ? C32 C31 O12 C25 175.1(5) . . . . ? O14 C44 O13 Zn2 -1.7(7) . . . 3_556 ? C43 C44 O13 Zn2 -179.4(3) . . . 3_556 ? O13 C44 O14 Zn1 21.1(7) . . . 3_556 ? C43 C44 O14 Zn1 -161.2(3) . . . 3_556 ? O4 Zn3 O15 Zn1 113.61(19) 2_445 . . . ? O11 Zn3 O15 Zn1 -108.58(19) 2 . . . ? O9 Zn3 O15 Zn1 4.34(19) . . . . ? O4 Zn3 O15 Zn2 -131.56(18) 2_445 . . . ? O11 Zn3 O15 Zn2 6.3(2) 2 . . . ? O9 Zn3 O15 Zn2 119.17(18) . . . . ? O14 Zn1 O15 Zn3 82.5(2) 3_556 . . . ? O8 Zn1 O15 Zn3 -37.5(2) . . . . ? O1 Zn1 O15 Zn3 -156.77(17) . . . . ? Zn2 Zn1 O15 Zn3 124.9(2) . . . . ? O14 Zn1 O15 Zn2 -42.44(18) 3_556 . . . ? O8 Zn1 O15 Zn2 -162.39(14) . . . . ? O1 Zn1 O15 Zn2 78.30(16) . . . . ? O13 Zn2 O15 Zn3 -95.26(19) 3_556 . . . ? O10 Zn2 O15 Zn3 -7.1(2) 2 . . . ? O6 Zn2 O15 Zn3 99.7(3) 4_665 . . . ? O2 Zn2 O15 Zn3 178.3(2) . . . . ? O7 Zn2 O15 Zn3 80.26(19) 4_665 . . . ? C22 Zn2 O15 Zn3 87.2(2) 4_665 . . . ? Zn1 Zn2 O15 Zn3 -124.2(2) . . . . ? O13 Zn2 O15 Zn1 28.93(18) 3_556 . . . ? O10 Zn2 O15 Zn1 117.09(17) 2 . . . ? O6 Zn2 O15 Zn1 -136.2(2) 4_665 . . . ? O2 Zn2 O15 Zn1 -57.56(16) . . . . ? O7 Zn2 O15 Zn1 -155.56(15) 4_665 . . . ? C22 Zn2 O15 Zn1 -148.62(14) 4_665 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15 H15O O3 0.837(19) 2.06(3) 2.801(5) 147(5) 2_445 O1W H1A O4 0.88(2) 2.01(18) 2.72(3) 142 3_456 O1W H1A O3 0.88(2) 2.57(9) 3.41(3) 160(21) 3_456 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.452 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 938334' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 N4 O16 Zn3' _chemical_formula_sum 'C52 H40 N4 O16 Zn3' _chemical_formula_weight 1173.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 9.842(2) _cell_length_b 12.262(3) _cell_length_c 20.186(4) _cell_angle_alpha 90 _cell_angle_beta 97.577(19) _cell_angle_gamma 90 _cell_volume 2414.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1666 _cell_measurement_theta_min 2.9464 _cell_measurement_theta_max 29.2257 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6523 _exptl_absorpt_correction_T_max 0.7159 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11452 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4218 _reflns_number_gt 3062 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1W---H1C and O1W---H1D were restrained to 0.87+-0.02 \%A. The distance of H1C...H1D was refined restrained to 1.44+-0.01 \%A. For C19, C26, O1, O2, O3, O5 and O6, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. For C22 and O6, some anisotropic displacement ellipsoids were rather elongated which led us to use the DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+3.7099P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4218 _refine_ls_number_parameters 345 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.2500 0.82246(8) -0.2500 0.0158(3) Uani 1 2 d S . . Zn2 Zn 0.02808(6) 0.61484(5) -0.17735(3) 0.0172(2) Uani 1 1 d D . . C1 C -0.3266(8) 0.6494(8) -0.0670(4) 0.050(2) Uani 1 1 d . . . C2 C -0.2549(9) 0.5739(8) -0.0241(4) 0.055(2) Uani 1 1 d . . . H2 H -0.1782 0.5392 -0.0366 0.066 Uiso 1 1 calc R . . C3 C -0.2974(8) 0.5508(8) 0.0364(4) 0.051(2) Uani 1 1 d . . . C4 C -0.4146(9) 0.5988(8) 0.0535(4) 0.056(2) Uani 1 1 d . . . H4 H -0.4446 0.5814 0.0940 0.068 Uiso 1 1 calc R . . C5 C -0.4872(8) 0.6716(7) 0.0115(4) 0.049(2) Uani 1 1 d . . . C6 C -0.4454(9) 0.6978(8) -0.0477(4) 0.055(2) Uani 1 1 d . . . H6 H -0.4952 0.7479 -0.0757 0.067 Uiso 1 1 calc R . . C7 C -0.2829(8) 0.6758(8) -0.1330(4) 0.052(2) Uani 1 1 d . . . C8 C -0.2147(9) 0.4761(8) 0.0858(4) 0.050(2) Uani 1 1 d . . . C9 C -0.6833(10) 0.7890(9) -0.0086(4) 0.066(3) Uani 1 1 d . . . H9A H -0.7209 0.7524 -0.0496 0.079 Uiso 1 1 calc R . . H9B H -0.6270 0.8493 -0.0201 0.079 Uiso 1 1 calc R . . C10 C -0.7963(9) 0.8303(9) 0.0270(4) 0.057(2) Uani 1 1 d . . . C11 C -0.9010(10) 0.7609(9) 0.0416(5) 0.065(3) Uani 1 1 d . . . H11 H -0.8974 0.6874 0.0306 0.078 Uiso 1 1 calc R . . C12 C -1.0080(10) 0.7981(9) 0.0716(4) 0.062(2) Uani 1 1 d . . . H12 H -1.0757 0.7498 0.0811 0.075 Uiso 1 1 calc R . . C13 C -1.0172(9) 0.9107(8) 0.0886(4) 0.050(2) Uani 1 1 d . . . C14 C -0.9147(9) 0.9801(8) 0.0726(4) 0.055(2) Uani 1 1 d . . . H14 H -0.9202 1.0544 0.0809 0.066 Uiso 1 1 calc R . . C15 C -0.8052(9) 0.9396(9) 0.0445(4) 0.058(2) Uani 1 1 d . . . H15 H -0.7348 0.9868 0.0369 0.070 Uiso 1 1 calc R . . C16 C -1.1405(8) 0.9543(8) 0.1149(4) 0.051(2) Uani 1 1 d . . . C17 C -1.2656(10) 0.9043(9) 0.0972(5) 0.066(3) Uani 1 1 d . . . H17 H -1.2679 0.8403 0.0723 0.079 Uiso 1 1 calc R . . C18 C -1.3867(10) 0.9437(11) 0.1141(5) 0.075(3) Uani 1 1 d . . . H18 H -1.4690 0.9075 0.1013 0.090 Uiso 1 1 calc R . . C19 C -1.3822(11) 1.0422(11) 0.1519(5) 0.075(3) Uani 1 1 d U . . H19 H -1.4623 1.0706 0.1648 0.090 Uiso 1 1 calc R . . C20 C -1.2629(11) 1.0938(9) 0.1690(5) 0.068(3) Uani 1 1 d . . . H20 H -1.2622 1.1599 0.1916 0.082 Uiso 1 1 calc R . . C21 C -1.1379(9) 1.0502(8) 0.1534(4) 0.056(2) Uani 1 1 d . . . C22 C -1.0117(10) 1.1066(9) 0.1824(4) 0.056(2) Uani 1 1 d U . . C23 C 0.0529(14) 0.3906(12) -0.2589(6) 0.092(4) Uani 1 1 d . . . H23 H 0.1246 0.4178 -0.2797 0.111 Uiso 1 1 calc R . . C24 C 0.0030(14) 0.2866(14) -0.2640(7) 0.105(4) Uani 1 1 d . . . H24 H 0.0333 0.2303 -0.2893 0.126 Uiso 1 1 calc R . . C25 C -0.1106(11) 0.3813(8) -0.2001(5) 0.062(3) Uani 1 1 d . . . H25 H -0.1755 0.4015 -0.1728 0.075 Uiso 1 1 calc R . . C26 C -0.1906(12) 0.1908(11) -0.2214(6) 0.085(3) Uani 1 1 d U . . H26A H -0.2272 0.1930 -0.1791 0.102 Uiso 1 1 calc R . . H26B H -0.1390 0.1236 -0.2228 0.102 Uiso 1 1 calc R . . N1 N -0.0195(9) 0.4467(7) -0.2185(4) 0.066(2) Uani 1 1 d . . . N2 N -0.1004(10) 0.2813(7) -0.2249(4) 0.073(2) Uani 1 1 d . . . O1 O -0.3405(6) 0.7572(6) -0.1637(3) 0.0645(17) Uani 1 1 d U . . O2 O -0.1934(7) 0.6189(6) -0.1549(3) 0.0655(17) Uani 1 1 d U . . O3 O -0.0981(7) 0.4457(6) 0.0720(3) 0.0699(18) Uani 1 1 d U . . O4 O -0.2572(6) 0.4486(6) 0.1383(3) 0.0695(19) Uani 1 1 d . . . O5 O -0.6020(7) 0.7142(6) 0.0347(3) 0.0689(18) Uani 1 1 d U . . O6 O -0.9988(9) 1.2058(7) 0.1736(4) 0.097(2) Uani 1 1 d U . . O7 O -0.9188(7) 1.0558(6) 0.2181(3) 0.0700(19) Uani 1 1 d . . . O1W O 0.0922(7) 0.6702(7) -0.2800(3) 0.0700(19) Uani 1 1 d D . . H1C H 0.033(9) 0.699(7) -0.312(4) 0.105 Uiso 1 1 d D . . H1D H 0.084(10) 0.5996(18) -0.279(2) 0.105 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0167(5) 0.0178(5) 0.0134(5) 0.000 0.0042(3) 0.000 Zn2 0.0191(4) 0.0153(4) 0.0175(4) 0.0032(2) 0.0032(3) 0.0043(3) C1 0.043(5) 0.051(5) 0.056(5) 0.003(4) 0.009(4) 0.005(4) C2 0.062(6) 0.056(6) 0.047(5) 0.006(4) 0.012(4) 0.014(5) C3 0.047(5) 0.054(6) 0.050(5) 0.001(4) 0.003(4) -0.002(4) C4 0.059(6) 0.066(7) 0.046(5) 0.008(4) 0.016(4) 0.003(5) C5 0.047(5) 0.055(6) 0.046(5) 0.003(4) 0.013(4) 0.016(4) C6 0.059(5) 0.055(6) 0.053(5) 0.003(4) 0.005(4) 0.014(5) C7 0.043(5) 0.064(6) 0.052(5) 0.013(4) 0.012(4) 0.024(4) C8 0.055(5) 0.049(6) 0.049(5) -0.001(4) 0.017(4) -0.002(4) C9 0.063(6) 0.079(8) 0.055(5) 0.006(5) 0.006(4) 0.025(6) C10 0.053(5) 0.066(7) 0.052(5) -0.007(4) 0.013(4) 0.009(5) C11 0.077(7) 0.055(6) 0.065(6) -0.013(5) 0.015(5) 0.003(5) C12 0.068(6) 0.060(7) 0.060(5) -0.011(5) 0.015(5) 0.005(5) C13 0.050(5) 0.047(5) 0.054(5) -0.006(4) 0.007(4) -0.001(4) C14 0.055(5) 0.056(6) 0.056(5) -0.001(4) 0.011(4) 0.006(5) C15 0.059(6) 0.066(7) 0.049(5) 0.001(4) 0.009(4) 0.005(5) C16 0.043(5) 0.061(6) 0.050(5) 0.000(4) 0.005(4) 0.009(4) C17 0.052(6) 0.077(8) 0.070(6) -0.006(5) 0.011(5) -0.007(5) C18 0.047(6) 0.111(10) 0.066(6) 0.013(6) 0.003(4) 0.000(6) C19 0.069(5) 0.085(5) 0.074(4) 0.004(4) 0.018(4) 0.006(4) C20 0.071(7) 0.073(8) 0.059(6) 0.001(5) 0.004(5) 0.013(6) C21 0.060(6) 0.061(6) 0.050(5) 0.001(4) 0.012(4) 0.004(5) C22 0.063(6) 0.060(4) 0.047(5) -0.011(4) 0.014(4) 0.003(5) C23 0.102(9) 0.093(11) 0.089(8) -0.030(7) 0.039(7) -0.016(8) C24 0.107(10) 0.106(12) 0.102(9) -0.039(8) 0.020(8) 0.006(9) C25 0.080(7) 0.044(6) 0.062(6) -0.007(4) 0.004(5) -0.005(5) C26 0.092(5) 0.072(5) 0.087(5) 0.003(4) -0.006(4) -0.004(4) N1 0.074(5) 0.065(6) 0.061(5) -0.014(4) 0.019(4) -0.004(5) N2 0.089(6) 0.047(5) 0.082(6) -0.009(4) 0.004(5) 0.000(5) O1 0.0643(18) 0.0649(19) 0.0644(18) 0.0020(10) 0.0088(10) 0.0008(10) O2 0.0652(19) 0.066(2) 0.0655(19) 0.0001(10) 0.0103(10) 0.0004(10) O3 0.071(3) 0.078(4) 0.061(3) 0.002(3) 0.009(3) 0.021(3) O4 0.065(4) 0.082(5) 0.064(4) 0.022(4) 0.018(3) 0.004(4) O5 0.069(3) 0.079(4) 0.061(3) 0.008(3) 0.019(3) 0.018(3) O6 0.116(4) 0.062(3) 0.117(4) -0.002(3) 0.026(4) -0.001(4) O7 0.070(4) 0.076(5) 0.061(4) -0.007(3) -0.003(3) -0.011(4) O1W 0.064(4) 0.075(5) 0.072(4) 0.016(3) 0.012(3) 0.003(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.208(6) 2_454 ? Zn1 O1 2.208(6) . ? Zn1 O7 2.264(7) 3_475 ? Zn1 O7 2.264(7) 4_675 ? Zn2 O6 2.221(9) 3_475 ? Zn2 N1 2.249(9) . ? Zn2 O3 2.273(6) 3_565 ? Zn2 O2 2.285(7) . ? Zn2 O1W 2.344(7) . ? Zn2 O4 2.417(6) 3_565 ? C1 C2 1.394(12) . ? C1 C6 1.411(12) . ? C1 C7 1.489(12) . ? C2 C3 1.373(11) . ? C2 H2 0.9300 . ? C3 C4 1.378(12) . ? C3 C8 1.510(12) . ? C4 C5 1.366(12) . ? C4 H4 0.9300 . ? C5 C6 1.352(11) . ? C5 O5 1.382(10) . ? C6 H6 0.9300 . ? C7 O2 1.249(10) . ? C7 O1 1.268(10) . ? C8 O4 1.236(10) . ? C8 O3 1.272(10) . ? C9 O5 1.437(11) . ? C9 C10 1.491(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.392(14) . ? C10 C11 1.397(14) . ? C11 C12 1.361(13) . ? C11 H11 0.9300 . ? C12 C13 1.429(13) . ? C12 H12 0.9300 . ? C13 C14 1.389(12) . ? C13 C16 1.487(12) . ? C14 C15 1.375(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.380(13) . ? C16 C21 1.407(13) . ? C17 C18 1.370(14) . ? C17 H17 0.9300 . ? C18 C19 1.427(17) . ? C18 H18 0.9300 . ? C19 C20 1.337(15) . ? C19 H19 0.9300 . ? C20 C21 1.414(13) . ? C20 H20 0.9300 . ? C21 C22 1.475(13) . ? C22 O6 1.238(12) . ? C22 O7 1.253(11) . ? C23 N1 1.341(14) . ? C23 C24 1.365(19) . ? C23 H23 0.9300 . ? C24 N2 1.370(15) . ? C24 H24 0.9300 . ? C25 N1 1.293(12) . ? C25 N2 1.333(12) . ? C25 H25 0.9300 . ? C26 N2 1.428(15) . ? C26 C26 1.53(2) 2_454 ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? O3 Zn2 2.273(6) 3_565 ? O4 Zn2 2.417(6) 3_565 ? O6 Zn2 2.221(9) 3_475 ? O7 Zn1 2.264(7) 3_475 ? O1W H1C 0.88(2) . ? O1W H1D 0.87(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 137.5(4) 2_454 . ? O1 Zn1 O7 96.1(2) 2_454 3_475 ? O1 Zn1 O7 111.8(2) . 3_475 ? O1 Zn1 O7 111.8(2) 2_454 4_675 ? O1 Zn1 O7 96.1(2) . 4_675 ? O7 Zn1 O7 97.4(4) 3_475 4_675 ? O6 Zn2 N1 154.0(3) 3_475 . ? O6 Zn2 O3 108.5(3) 3_475 3_565 ? N1 Zn2 O3 93.9(3) . 3_565 ? O6 Zn2 O2 80.8(3) 3_475 . ? N1 Zn2 O2 86.3(3) . . ? O3 Zn2 O2 90.1(2) 3_565 . ? O6 Zn2 O1W 78.1(3) 3_475 . ? N1 Zn2 O1W 90.4(3) . . ? O3 Zn2 O1W 146.9(2) 3_565 . ? O2 Zn2 O1W 123.0(2) . . ? O6 Zn2 O4 115.3(3) 3_475 3_565 ? N1 Zn2 O4 88.0(3) . 3_565 ? O3 Zn2 O4 55.6(2) 3_565 3_565 ? O2 Zn2 O4 144.6(2) . 3_565 ? O1W Zn2 O4 91.9(2) . 3_565 ? C2 C1 C6 118.5(8) . . ? C2 C1 C7 121.2(7) . . ? C6 C1 C7 120.3(7) . . ? C3 C2 C1 120.1(8) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.9(8) . . ? C2 C3 C8 120.8(8) . . ? C4 C3 C8 119.3(7) . . ? C5 C4 C3 120.7(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.6(8) . . ? C6 C5 O5 124.6(7) . . ? C4 C5 O5 114.8(7) . . ? C5 C6 C1 120.2(8) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? O2 C7 O1 123.9(8) . . ? O2 C7 C1 119.7(8) . . ? O1 C7 C1 116.4(7) . . ? O4 C8 O3 121.7(8) . . ? O4 C8 C3 121.2(8) . . ? O3 C8 C3 117.1(7) . . ? O5 C9 C10 108.3(7) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C15 C10 C11 117.4(8) . . ? C15 C10 C9 121.6(9) . . ? C11 C10 C9 120.9(9) . . ? C12 C11 C10 121.7(10) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 120.5(9) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 117.7(8) . . ? C14 C13 C16 121.0(8) . . ? C12 C13 C16 120.9(8) . . ? C15 C14 C13 120.5(9) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C10 122.0(9) . . ? C14 C15 H15 119.0 . . ? C10 C15 H15 119.0 . . ? C17 C16 C21 117.7(8) . . ? C17 C16 C13 119.4(8) . . ? C21 C16 C13 122.8(8) . . ? C18 C17 C16 123.7(11) . . ? C18 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? C17 C18 C19 117.7(10) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C20 C19 C18 120.2(10) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.6(11) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C16 C21 C20 119.1(9) . . ? C16 C21 C22 124.4(8) . . ? C20 C21 C22 116.5(9) . . ? O6 C22 O7 119.4(9) . . ? O6 C22 C21 120.1(10) . . ? O7 C22 C21 120.5(9) . . ? N1 C23 C24 108.1(11) . . ? N1 C23 H23 126.0 . . ? C24 C23 H23 126.0 . . ? C23 C24 N2 106.7(11) . . ? C23 C24 H24 126.6 . . ? N2 C24 H24 126.6 . . ? N1 C25 N2 111.9(10) . . ? N1 C25 H25 124.0 . . ? N2 C25 H25 124.0 . . ? N2 C26 C26 112.3(8) . 2_454 ? N2 C26 H26A 109.1 . . ? C26 C26 H26A 109.1 2_454 . ? N2 C26 H26B 109.1 . . ? C26 C26 H26B 109.1 2_454 . ? H26A C26 H26B 107.9 . . ? C25 N1 C23 107.5(10) . . ? C25 N1 Zn2 125.5(7) . . ? C23 N1 Zn2 126.4(8) . . ? C25 N2 C24 105.7(10) . . ? C25 N2 C26 128.1(11) . . ? C24 N2 C26 125.4(11) . . ? C7 O1 Zn1 118.0(5) . . ? C7 O2 Zn2 144.9(6) . . ? C8 O3 Zn2 93.5(5) . 3_565 ? C8 O4 Zn2 87.8(5) . 3_565 ? C5 O5 C9 116.7(6) . . ? C22 O6 Zn2 162.1(8) . 3_475 ? C22 O7 Zn1 106.7(7) . 3_475 ? Zn2 O1W H1C 122(8) . . ? Zn2 O1W H1D 70.1(15) . . ? H1C O1W H1D 111(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.2(14) . . . . ? C7 C1 C2 C3 -179.9(9) . . . . ? C1 C2 C3 C4 2.9(14) . . . . ? C1 C2 C3 C8 -175.1(8) . . . . ? C2 C3 C4 C5 -1.8(14) . . . . ? C8 C3 C4 C5 176.2(9) . . . . ? C3 C4 C5 C6 0.1(15) . . . . ? C3 C4 C5 O5 -179.6(8) . . . . ? C4 C5 C6 C1 0.5(14) . . . . ? O5 C5 C6 C1 -179.8(9) . . . . ? C2 C1 C6 C5 0.5(14) . . . . ? C7 C1 C6 C5 178.2(9) . . . . ? C2 C1 C7 O2 10.5(14) . . . . ? C6 C1 C7 O2 -167.1(9) . . . . ? C2 C1 C7 O1 -169.2(9) . . . . ? C6 C1 C7 O1 13.2(13) . . . . ? C2 C3 C8 O4 -174.7(9) . . . . ? C4 C3 C8 O4 7.2(13) . . . . ? C2 C3 C8 O3 7.5(13) . . . . ? C4 C3 C8 O3 -170.5(8) . . . . ? O5 C9 C10 C15 115.2(10) . . . . ? O5 C9 C10 C11 -67.5(11) . . . . ? C15 C10 C11 C12 0.2(14) . . . . ? C9 C10 C11 C12 -177.2(9) . . . . ? C10 C11 C12 C13 0.6(14) . . . . ? C11 C12 C13 C14 0.9(13) . . . . ? C11 C12 C13 C16 173.7(8) . . . . ? C12 C13 C14 C15 -3.2(12) . . . . ? C16 C13 C14 C15 -176.0(8) . . . . ? C13 C14 C15 C10 4.2(13) . . . . ? C11 C10 C15 C14 -2.6(13) . . . . ? C9 C10 C15 C14 174.7(8) . . . . ? C14 C13 C16 C17 144.7(9) . . . . ? C12 C13 C16 C17 -27.9(12) . . . . ? C14 C13 C16 C21 -30.3(12) . . . . ? C12 C13 C16 C21 157.1(9) . . . . ? C21 C16 C17 C18 1.0(15) . . . . ? C13 C16 C17 C18 -174.2(9) . . . . ? C16 C17 C18 C19 0.3(15) . . . . ? C17 C18 C19 C20 0.9(15) . . . . ? C18 C19 C20 C21 -3.4(15) . . . . ? C17 C16 C21 C20 -3.3(13) . . . . ? C13 C16 C21 C20 171.7(8) . . . . ? C17 C16 C21 C22 173.2(9) . . . . ? C13 C16 C21 C22 -11.8(14) . . . . ? C19 C20 C21 C16 4.6(14) . . . . ? C19 C20 C21 C22 -172.2(9) . . . . ? C16 C21 C22 O6 129.3(10) . . . . ? C20 C21 C22 O6 -54.1(12) . . . . ? C16 C21 C22 O7 -53.2(12) . . . . ? C20 C21 C22 O7 123.4(10) . . . . ? N1 C23 C24 N2 -0.8(15) . . . . ? N2 C25 N1 C23 1.9(12) . . . . ? N2 C25 N1 Zn2 -169.7(6) . . . . ? C24 C23 N1 C25 -0.7(14) . . . . ? C24 C23 N1 Zn2 170.8(9) . . . . ? O6 Zn2 N1 C25 -87.5(11) 3_475 . . . ? O3 Zn2 N1 C25 62.5(9) 3_565 . . . ? O2 Zn2 N1 C25 -27.3(8) . . . . ? O1W Zn2 N1 C25 -150.3(9) . . . . ? O4 Zn2 N1 C25 117.8(9) 3_565 . . . ? O6 Zn2 N1 C23 102.6(11) 3_475 . . . ? O3 Zn2 N1 C23 -107.5(10) 3_565 . . . ? O2 Zn2 N1 C23 162.7(10) . . . . ? O1W Zn2 N1 C23 39.7(10) . . . . ? O4 Zn2 N1 C23 -52.2(10) 3_565 . . . ? N1 C25 N2 C24 -2.3(12) . . . . ? N1 C25 N2 C26 -173.1(9) . . . . ? C23 C24 N2 C25 1.8(14) . . . . ? C23 C24 N2 C26 172.9(11) . . . . ? C26 C26 N2 C25 86.9(15) 2_454 . . . ? C26 C26 N2 C24 -82.1(15) 2_454 . . . ? O2 C7 O1 Zn1 -12.8(12) . . . . ? C1 C7 O1 Zn1 166.9(6) . . . . ? O1 Zn1 O1 C7 41.4(6) 2_454 . . . ? O7 Zn1 O1 C7 -85.9(7) 3_475 . . . ? O7 Zn1 O1 C7 173.5(7) 4_675 . . . ? O1 C7 O2 Zn2 70.5(14) . . . . ? C1 C7 O2 Zn2 -109.2(11) . . . . ? O6 Zn2 O2 C7 -19.5(10) 3_475 . . . ? N1 Zn2 O2 C7 -176.8(10) . . . . ? O3 Zn2 O2 C7 89.2(10) 3_565 . . . ? O1W Zn2 O2 C7 -88.8(10) . . . . ? O4 Zn2 O2 C7 101.9(10) 3_565 . . . ? O4 C8 O3 Zn2 -12.7(9) . . . 3_565 ? C3 C8 O3 Zn2 165.1(7) . . . 3_565 ? O3 C8 O4 Zn2 11.9(9) . . . 3_565 ? C3 C8 O4 Zn2 -165.8(8) . . . 3_565 ? C6 C5 O5 C9 1.8(14) . . . . ? C4 C5 O5 C9 -178.5(9) . . . . ? C10 C9 O5 C5 -176.6(8) . . . . ? O7 C22 O6 Zn2 -111(2) . . . 3_475 ? C21 C22 O6 Zn2 67(3) . . . 3_475 ? O6 C22 O7 Zn1 -2.4(10) . . . 3_475 ? C21 C22 O7 Zn1 -179.9(6) . . . 3_475 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1C O1 0.88(2) 2.02(7) 2.798(9) 146(11) 2_454 O1W H1D N1 0.87(2) 2.53(3) 3.259(12) 142(3) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.962 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.140 _database_code_depnum_ccdc_archive 'CCDC 938335' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Cd3 N4 O16' _chemical_formula_sum 'C52 H40 Cd3 N4 O16' _chemical_formula_weight 1314.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ' Monoclinic' _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 9.8520(4) _cell_length_b 12.2410(5) _cell_length_c 20.2090(8) _cell_angle_alpha 90 _cell_angle_beta 97.445(4) _cell_angle_gamma 90 _cell_volume 2416.63(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2820 _cell_measurement_theta_min 3.0436 _cell_measurement_theta_max 29.2213 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6652 _exptl_absorpt_correction_T_max 0.7594 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9252 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4258 _reflns_number_gt 3294 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1W---H1C and O1W---H1D were restrained to 0.87+-0.02 \%A. The distance of H1C...H1D were restrained to 1.44+-0.01 \%A. For C23 and C24, some anisotropic displacement ellipsoids were rather elongated which led us to use the SIMU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4258 _refine_ls_number_parameters 345 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.7500 0.32245(3) 0.7500 0.02230(12) Uani 1 2 d S . . Cd2 Cd 0.47200(3) 0.11484(2) 0.677367(15) 0.02362(9) Uani 1 1 d . . . C1 C 0.8279(4) 0.1485(3) 0.5668(2) 0.0235(10) Uani 1 1 d . . . C2 C 0.7544(4) 0.0755(3) 0.5242(2) 0.0246(10) Uani 1 1 d . . . H2 H 0.6761 0.0428 0.5365 0.030 Uiso 1 1 calc R . . C3 C 0.7973(4) 0.0509(3) 0.46290(19) 0.0240(9) Uani 1 1 d . . . C4 C 0.9151(4) 0.0974(3) 0.4461(2) 0.0268(10) Uani 1 1 d . . . H4 H 0.9456 0.0788 0.4059 0.032 Uiso 1 1 calc R . . C5 C 0.9888(4) 0.1713(3) 0.4881(2) 0.0278(10) Uani 1 1 d . . . C6 C 0.9446(4) 0.1985(3) 0.5484(2) 0.0271(10) Uani 1 1 d . . . H6 H 0.9924 0.2497 0.5763 0.033 Uiso 1 1 calc R . . C7 C 0.7818(4) 0.1765(3) 0.6330(2) 0.0263(10) Uani 1 1 d . . . C8 C 0.7137(4) -0.0238(3) 0.4151(2) 0.0263(10) Uani 1 1 d . . . C9 C 1.1822(4) 0.2897(4) 0.5089(2) 0.0352(11) Uani 1 1 d . . . H9A H 1.2183 0.2532 0.5500 0.042 Uiso 1 1 calc R . . H9B H 1.1262 0.3506 0.5197 0.042 Uiso 1 1 calc R . . C10 C 1.2976(4) 0.3298(4) 0.4731(2) 0.0306(11) Uani 1 1 d . . . C11 C 1.4022(4) 0.2607(3) 0.4592(2) 0.0335(11) Uani 1 1 d . . . H11 H 1.3998 0.1873 0.4708 0.040 Uiso 1 1 calc R . . C12 C 1.5090(4) 0.2995(3) 0.4285(2) 0.0321(11) Uani 1 1 d . . . H12 H 1.5765 0.2514 0.4185 0.039 Uiso 1 1 calc R . . C13 C 1.5180(4) 0.4100(3) 0.41210(19) 0.0238(9) Uani 1 1 d . . . C14 C 1.4146(4) 0.4790(3) 0.42747(19) 0.0258(10) Uani 1 1 d . . . H14 H 1.4193 0.5532 0.4182 0.031 Uiso 1 1 calc R . . C15 C 1.3049(4) 0.4393(4) 0.4562(2) 0.0297(10) Uani 1 1 d . . . H15 H 1.2350 0.4865 0.4643 0.036 Uiso 1 1 calc R . . C16 C 1.6404(4) 0.4533(3) 0.3847(2) 0.0248(10) Uani 1 1 d . . . C17 C 1.7672(4) 0.4036(4) 0.4039(2) 0.0367(11) Uani 1 1 d . . . H17 H 1.7710 0.3408 0.4300 0.044 Uiso 1 1 calc R . . C18 C 1.8870(4) 0.4451(4) 0.3850(2) 0.0467(13) Uani 1 1 d . . . H18 H 1.9695 0.4084 0.3962 0.056 Uiso 1 1 calc R . . C19 C 1.8829(5) 0.5414(5) 0.3495(2) 0.0473(14) Uani 1 1 d . . . H19 H 1.9634 0.5714 0.3380 0.057 Uiso 1 1 calc R . . C20 C 1.7604(4) 0.5933(4) 0.3311(2) 0.0380(12) Uani 1 1 d . . . H20 H 1.7588 0.6590 0.3079 0.046 Uiso 1 1 calc R . . C21 C 1.6390(4) 0.5490(3) 0.34666(19) 0.0247(10) Uani 1 1 d . . . C22 C 1.5106(4) 0.6074(3) 0.3173(2) 0.0309(11) Uani 1 1 d . . . C23 C 0.4459(5) -0.1127(5) 0.7583(3) 0.0625(15) Uani 1 1 d U . . H23 H 0.3729 -0.0868 0.7787 0.075 Uiso 1 1 calc R . . C24 C 0.4950(6) -0.2146(5) 0.7635(3) 0.0657(16) Uani 1 1 d U . . H24 H 0.4633 -0.2715 0.7879 0.079 Uiso 1 1 calc R . . C25 C 0.6109(5) -0.1197(4) 0.7001(2) 0.0373(11) Uani 1 1 d . . . H25 H 0.6752 -0.1007 0.6722 0.045 Uiso 1 1 calc R . . C26 C 0.6923(5) -0.3108(4) 0.7218(3) 0.0562(14) Uani 1 1 d . . . H26A H 0.7296 -0.3073 0.6797 0.067 Uiso 1 1 calc R . . H26B H 0.6413 -0.3785 0.7226 0.067 Uiso 1 1 calc R . . N1 N 0.5194(4) -0.0523(3) 0.71837(18) 0.0383(10) Uani 1 1 d . . . N2 N 0.6003(4) -0.2190(3) 0.72625(19) 0.0439(10) Uani 1 1 d . . . O1 O 0.6933(3) 0.1189(2) 0.65467(14) 0.0356(8) Uani 1 1 d . . . O2 O 0.8412(3) 0.2572(2) 0.66510(14) 0.0346(8) Uani 1 1 d . . . O3 O 0.5990(3) -0.0537(2) 0.42810(14) 0.0378(8) Uani 1 1 d . . . O4 O 0.7567(3) -0.0509(2) 0.36117(14) 0.0365(8) Uani 1 1 d . . . O5 O 1.1021(3) 0.2151(2) 0.46522(14) 0.0401(8) Uani 1 1 d . . . O6 O 1.4183(3) 0.5555(3) 0.28213(15) 0.0389(8) Uani 1 1 d . . . O7 O 1.4984(4) 0.7068(2) 0.32777(19) 0.0641(11) Uani 1 1 d . . . O1W O 0.4074(3) 0.1679(3) 0.77919(14) 0.0388(8) Uani 1 1 d D . . H1C H 0.366(4) 0.131(3) 0.8063(15) 0.058 Uiso 1 1 d D . . H1D H 0.477(3) 0.204(3) 0.7976(17) 0.058 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0229(2) 0.0241(2) 0.0205(3) 0.000 0.00499(18) 0.000 Cd2 0.02480(16) 0.02204(17) 0.02422(18) -0.00322(14) 0.00397(13) -0.00425(14) C1 0.022(2) 0.025(2) 0.024(2) -0.0023(19) 0.0029(18) -0.0022(18) C2 0.016(2) 0.027(2) 0.030(3) -0.002(2) 0.0029(18) -0.0070(18) C3 0.028(2) 0.024(2) 0.020(2) -0.005(2) 0.0020(18) -0.003(2) C4 0.028(2) 0.030(2) 0.023(2) -0.003(2) 0.0070(19) -0.005(2) C5 0.025(2) 0.034(2) 0.025(3) 0.001(2) 0.0061(19) -0.005(2) C6 0.028(2) 0.029(2) 0.025(3) -0.007(2) 0.0029(19) -0.008(2) C7 0.019(2) 0.035(3) 0.024(3) 0.002(2) 0.0011(19) 0.003(2) C8 0.028(2) 0.026(2) 0.025(3) 0.001(2) 0.003(2) 0.000(2) C9 0.038(3) 0.041(3) 0.028(3) -0.005(2) 0.009(2) -0.019(2) C10 0.029(2) 0.041(3) 0.022(3) -0.003(2) 0.0038(19) -0.012(2) C11 0.040(3) 0.026(2) 0.035(3) 0.010(2) 0.004(2) -0.007(2) C12 0.031(2) 0.027(2) 0.039(3) 0.005(2) 0.008(2) 0.002(2) C13 0.023(2) 0.028(2) 0.020(2) 0.003(2) 0.0000(17) -0.0006(19) C14 0.027(2) 0.027(2) 0.023(2) 0.004(2) -0.0007(18) -0.005(2) C15 0.025(2) 0.036(3) 0.027(3) -0.006(2) 0.0030(19) -0.003(2) C16 0.021(2) 0.030(2) 0.023(2) -0.003(2) 0.0035(18) -0.005(2) C17 0.027(2) 0.047(3) 0.035(3) 0.003(2) 0.001(2) 0.001(2) C18 0.026(2) 0.073(4) 0.042(3) -0.005(3) 0.004(2) 0.008(3) C19 0.033(3) 0.076(4) 0.035(3) -0.011(3) 0.015(2) -0.017(3) C20 0.039(3) 0.043(3) 0.033(3) -0.002(2) 0.009(2) -0.018(2) C21 0.030(2) 0.025(2) 0.018(2) -0.006(2) 0.0028(18) -0.006(2) C22 0.039(3) 0.025(2) 0.033(3) 0.009(2) 0.019(2) -0.002(2) C23 0.066(3) 0.061(4) 0.065(4) 0.026(3) 0.024(3) 0.006(3) C24 0.073(4) 0.056(4) 0.071(4) 0.030(3) 0.021(3) -0.006(3) C25 0.053(3) 0.028(3) 0.030(3) 0.004(2) 0.003(2) -0.003(2) C26 0.081(4) 0.021(3) 0.059(4) -0.001(3) -0.020(3) -0.001(3) N1 0.042(2) 0.034(2) 0.041(3) 0.010(2) 0.0116(19) -0.002(2) N2 0.063(3) 0.021(2) 0.044(3) 0.0046(19) -0.008(2) 0.001(2) O1 0.0271(15) 0.0451(19) 0.0375(19) 0.0000(16) 0.0154(14) -0.0064(15) O2 0.0291(16) 0.049(2) 0.0269(18) -0.0158(16) 0.0091(13) -0.0089(15) O3 0.0366(17) 0.048(2) 0.0298(19) -0.0076(15) 0.0068(14) -0.0240(16) O4 0.0339(16) 0.0427(18) 0.0337(19) -0.0177(16) 0.0073(14) -0.0036(15) O5 0.0381(17) 0.056(2) 0.0286(19) -0.0153(16) 0.0157(15) -0.0268(16) O6 0.0333(17) 0.0398(19) 0.042(2) 0.0065(16) -0.0005(15) 0.0082(16) O7 0.094(3) 0.0160(18) 0.090(3) 0.0036(19) 0.041(2) -0.0003(19) O1W 0.0347(18) 0.052(2) 0.0321(19) -0.0073(17) 0.0118(15) -0.0148(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.188(2) 2_656 ? Cd1 O2 2.188(2) . ? Cd1 O6 2.264(3) 4_566 ? Cd1 O6 2.264(3) 3_766 ? Cd2 O7 2.207(3) 3_766 ? Cd2 N1 2.234(4) . ? Cd2 O3 2.281(3) 3_656 ? Cd2 O1 2.285(2) . ? Cd2 O1W 2.324(3) . ? Cd2 O4 2.417(3) 3_656 ? Cd2 C8 2.682(4) 3_656 ? C1 C2 1.378(5) . ? C1 C6 1.396(5) . ? C1 C7 1.507(5) . ? C2 C3 1.394(5) . ? C2 H2 0.9300 . ? C3 C4 1.374(5) . ? C3 C8 1.497(5) . ? C4 C5 1.380(5) . ? C4 H4 0.9300 . ? C5 O5 1.371(4) . ? C5 C6 1.387(5) . ? C6 H6 0.9300 . ? C7 O1 1.244(4) . ? C7 O2 1.281(5) . ? C8 O3 1.247(4) . ? C8 O4 1.264(4) . ? C8 Cd2 2.682(4) 3_656 ? C9 O5 1.433(5) . ? C9 C10 1.506(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.387(6) . ? C10 C11 1.390(5) . ? C11 C12 1.374(5) . ? C11 H11 0.9300 . ? C12 C13 1.398(5) . ? C12 H12 0.9300 . ? C13 C14 1.389(5) . ? C13 C16 1.488(5) . ? C14 C15 1.379(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.398(5) . ? C16 C21 1.400(5) . ? C17 C18 1.383(5) . ? C17 H17 0.9300 . ? C18 C19 1.379(6) . ? C18 H18 0.9300 . ? C19 C20 1.372(6) . ? C19 H19 0.9300 . ? C20 C21 1.386(5) . ? C20 H20 0.9300 . ? C21 C22 1.507(6) . ? C22 O7 1.243(5) . ? C22 O6 1.252(5) . ? C23 C24 1.337(7) . ? C23 N1 1.369(5) . ? C23 H23 0.9300 . ? C24 N2 1.359(6) . ? C24 H24 0.9300 . ? C25 N1 1.310(5) . ? C25 N2 1.335(5) . ? C25 H25 0.9300 . ? C26 N2 1.455(5) . ? C26 C26 1.501(9) 2_656 ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? O3 Cd2 2.281(3) 3_656 ? O4 Cd2 2.417(3) 3_656 ? O6 Cd1 2.264(3) 3_766 ? O7 Cd2 2.207(3) 3_766 ? O1W H1C 0.853(10) . ? O1W H1D 0.853(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 137.20(16) 2_656 . ? O2 Cd1 O6 112.09(11) 2_656 4_566 ? O2 Cd1 O6 96.06(10) . 4_566 ? O2 Cd1 O6 96.06(10) 2_656 3_766 ? O2 Cd1 O6 112.09(11) . 3_766 ? O6 Cd1 O6 97.42(16) 4_566 3_766 ? O7 Cd2 N1 154.29(15) 3_766 . ? O7 Cd2 O3 107.87(13) 3_766 3_656 ? N1 Cd2 O3 94.03(13) . 3_656 ? O7 Cd2 O1 80.44(11) 3_766 . ? N1 Cd2 O1 86.30(11) . . ? O3 Cd2 O1 90.26(10) 3_656 . ? O7 Cd2 O1W 79.52(12) 3_766 . ? N1 Cd2 O1W 89.74(13) . . ? O3 Cd2 O1W 146.38(10) 3_656 . ? O1 Cd2 O1W 123.33(10) . . ? O7 Cd2 O4 115.37(12) 3_766 3_656 ? N1 Cd2 O4 87.95(11) . 3_656 ? O3 Cd2 O4 55.43(9) 3_656 3_656 ? O1 Cd2 O4 144.69(10) . 3_656 ? O1W Cd2 O4 91.42(9) . 3_656 ? O7 Cd2 C8 117.42(14) 3_766 3_656 ? N1 Cd2 C8 88.22(13) . 3_656 ? O3 Cd2 C8 27.62(9) 3_656 3_656 ? O1 Cd2 C8 116.82(11) . 3_656 ? O1W Cd2 C8 119.52(11) . 3_656 ? O4 Cd2 C8 28.10(9) 3_656 3_656 ? C2 C1 C6 120.1(4) . . ? C2 C1 C7 120.5(3) . . ? C6 C1 C7 119.4(4) . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 C8 120.4(3) . . ? C2 C3 C8 120.1(3) . . ? C3 C4 C5 120.9(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? O5 C5 C4 115.9(3) . . ? O5 C5 C6 124.3(4) . . ? C4 C5 C6 119.8(3) . . ? C5 C6 C1 119.5(4) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? O1 C7 O2 123.6(4) . . ? O1 C7 C1 119.3(4) . . ? O2 C7 C1 117.0(3) . . ? O3 C8 O4 121.2(4) . . ? O3 C8 C3 118.8(3) . . ? O4 C8 C3 119.9(3) . . ? O3 C8 Cd2 58.0(2) . 3_656 ? O4 C8 Cd2 64.2(2) . 3_656 ? C3 C8 Cd2 166.3(3) . 3_656 ? O5 C9 C10 107.6(3) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C15 C10 C11 118.3(3) . . ? C15 C10 C9 120.0(4) . . ? C11 C10 C9 121.6(4) . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 121.2(4) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 117.6(3) . . ? C14 C13 C16 121.3(4) . . ? C12 C13 C16 120.8(3) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 120.8(4) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C17 C16 C21 117.5(3) . . ? C17 C16 C13 118.7(4) . . ? C21 C16 C13 123.5(3) . . ? C18 C17 C16 121.8(4) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 120.3(4) . . ? C20 C21 C22 115.5(4) . . ? C16 C21 C22 124.1(3) . . ? O7 C22 O6 121.0(4) . . ? O7 C22 C21 119.5(4) . . ? O6 C22 C21 119.6(4) . . ? C24 C23 N1 109.7(4) . . ? C24 C23 H23 125.2 . . ? N1 C23 H23 125.2 . . ? C23 C24 N2 106.7(4) . . ? C23 C24 H24 126.6 . . ? N2 C24 H24 126.6 . . ? N1 C25 N2 111.7(4) . . ? N1 C25 H25 124.2 . . ? N2 C25 H25 124.2 . . ? N2 C26 C26 111.7(4) . 2_656 ? N2 C26 H26A 109.3 . . ? C26 C26 H26A 109.3 2_656 . ? N2 C26 H26B 109.3 . . ? C26 C26 H26B 109.3 2_656 . ? H26A C26 H26B 107.9 . . ? C25 N1 C23 105.2(4) . . ? C25 N1 Cd2 126.2(3) . . ? C23 N1 Cd2 127.8(3) . . ? C25 N2 C24 106.7(4) . . ? C25 N2 C26 126.7(4) . . ? C24 N2 C26 126.2(4) . . ? C7 O1 Cd2 144.4(3) . . ? C7 O2 Cd1 118.1(2) . . ? C8 O3 Cd2 94.4(2) . 3_656 ? C8 O4 Cd2 87.7(2) . 3_656 ? C5 O5 C9 116.7(3) . . ? C22 O6 Cd1 106.2(3) . 3_766 ? C22 O7 Cd2 160.7(3) . 3_766 ? Cd2 O1W H1C 129(3) . . ? Cd2 O1W H1D 104(3) . . ? H1C O1W H1D 114.3(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.6(6) . . . . ? C7 C1 C2 C3 179.5(4) . . . . ? C1 C2 C3 C4 1.8(6) . . . . ? C1 C2 C3 C8 -176.8(4) . . . . ? C2 C3 C4 C5 -2.4(6) . . . . ? C8 C3 C4 C5 176.2(4) . . . . ? C3 C4 C5 O5 -177.9(4) . . . . ? C3 C4 C5 C6 0.7(6) . . . . ? O5 C5 C6 C1 -179.8(4) . . . . ? C4 C5 C6 C1 1.7(6) . . . . ? C2 C1 C6 C5 -2.3(6) . . . . ? C7 C1 C6 C5 178.8(4) . . . . ? C2 C1 C7 O1 13.6(6) . . . . ? C6 C1 C7 O1 -167.5(4) . . . . ? C2 C1 C7 O2 -169.0(4) . . . . ? C6 C1 C7 O2 9.9(6) . . . . ? C4 C3 C8 O3 -171.1(4) . . . . ? C2 C3 C8 O3 7.6(6) . . . . ? C4 C3 C8 O4 5.4(6) . . . . ? C2 C3 C8 O4 -176.0(4) . . . . ? C4 C3 C8 Cd2 -98.6(11) . . . 3_656 ? C2 C3 C8 Cd2 80.1(12) . . . 3_656 ? O5 C9 C10 C15 115.4(4) . . . . ? O5 C9 C10 C11 -67.8(5) . . . . ? C15 C10 C11 C12 -1.0(7) . . . . ? C9 C10 C11 C12 -177.8(4) . . . . ? C10 C11 C12 C13 1.9(7) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C11 C12 C13 C16 174.2(4) . . . . ? C12 C13 C14 C15 -1.8(6) . . . . ? C16 C13 C14 C15 -176.5(4) . . . . ? C13 C14 C15 C10 2.7(6) . . . . ? C11 C10 C15 C14 -1.2(6) . . . . ? C9 C10 C15 C14 175.6(4) . . . . ? C14 C13 C16 C17 144.2(4) . . . . ? C12 C13 C16 C17 -30.3(6) . . . . ? C14 C13 C16 C21 -28.2(6) . . . . ? C12 C13 C16 C21 157.2(4) . . . . ? C21 C16 C17 C18 -1.4(6) . . . . ? C13 C16 C17 C18 -174.3(4) . . . . ? C16 C17 C18 C19 3.6(7) . . . . ? C17 C18 C19 C20 -2.3(7) . . . . ? C18 C19 C20 C21 -1.2(7) . . . . ? C19 C20 C21 C16 3.5(6) . . . . ? C19 C20 C21 C22 -173.7(4) . . . . ? C17 C16 C21 C20 -2.1(6) . . . . ? C13 C16 C21 C20 170.4(4) . . . . ? C17 C16 C21 C22 174.8(4) . . . . ? C13 C16 C21 C22 -12.7(6) . . . . ? C20 C21 C22 O7 -55.0(5) . . . . ? C16 C21 C22 O7 128.0(4) . . . . ? C20 C21 C22 O6 124.2(4) . . . . ? C16 C21 C22 O6 -52.8(6) . . . . ? N1 C23 C24 N2 -0.3(7) . . . . ? N2 C25 N1 C23 -0.3(6) . . . . ? N2 C25 N1 Cd2 -170.4(3) . . . . ? C24 C23 N1 C25 0.4(6) . . . . ? C24 C23 N1 Cd2 170.2(4) . . . . ? O7 Cd2 N1 C25 -86.4(5) 3_766 . . . ? O3 Cd2 N1 C25 62.4(4) 3_656 . . . ? O1 Cd2 N1 C25 -27.6(4) . . . . ? O1W Cd2 N1 C25 -151.0(4) . . . . ? O4 Cd2 N1 C25 117.5(4) 3_656 . . . ? C8 Cd2 N1 C25 89.4(4) 3_656 . . . ? O7 Cd2 N1 C23 105.8(5) 3_766 . . . ? O3 Cd2 N1 C23 -105.4(4) 3_656 . . . ? O1 Cd2 N1 C23 164.6(4) . . . . ? O1W Cd2 N1 C23 41.2(4) . . . . ? O4 Cd2 N1 C23 -50.2(4) 3_656 . . . ? C8 Cd2 N1 C23 -78.4(4) 3_656 . . . ? N1 C25 N2 C24 0.2(6) . . . . ? N1 C25 N2 C26 -173.8(4) . . . . ? C23 C24 N2 C25 0.1(6) . . . . ? C23 C24 N2 C26 174.1(5) . . . . ? C26 C26 N2 C25 89.2(7) 2_656 . . . ? C26 C26 N2 C24 -83.7(7) 2_656 . . . ? O2 C7 O1 Cd2 72.0(6) . . . . ? C1 C7 O1 Cd2 -110.8(4) . . . . ? O7 Cd2 O1 C7 -18.4(5) 3_766 . . . ? N1 Cd2 O1 C7 -176.2(5) . . . . ? O3 Cd2 O1 C7 89.7(5) 3_656 . . . ? O1W Cd2 O1 C7 -89.0(5) . . . . ? O4 Cd2 O1 C7 102.6(5) 3_656 . . . ? C8 Cd2 O1 C7 97.6(5) 3_656 . . . ? O1 C7 O2 Cd1 -15.4(5) . . . . ? C1 C7 O2 Cd1 167.3(3) . . . . ? O2 Cd1 O2 C7 43.1(3) 2_656 . . . ? O6 Cd1 O2 C7 175.3(3) 4_566 . . . ? O6 Cd1 O2 C7 -84.1(3) 3_766 . . . ? O4 C8 O3 Cd2 -11.8(4) . . . 3_656 ? C3 C8 O3 Cd2 164.6(3) . . . 3_656 ? O3 C8 O4 Cd2 11.1(4) . . . 3_656 ? C3 C8 O4 Cd2 -165.3(3) . . . 3_656 ? C4 C5 O5 C9 -178.3(4) . . . . ? C6 C5 O5 C9 3.2(6) . . . . ? C10 C9 O5 C5 -178.3(4) . . . . ? O7 C22 O6 Cd1 -0.5(5) . . . 3_766 ? C21 C22 O6 Cd1 -179.8(3) . . . 3_766 ? O6 C22 O7 Cd2 -106.5(11) . . . 3_766 ? C21 C22 O7 Cd2 72.7(13) . . . 3_766 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.574 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 938336' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H74 O40 Pb7' _chemical_formula_sum 'C88 H74 O40 Pb7' _chemical_formula_weight 3221.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1595(4) _cell_length_b 12.9301(4) _cell_length_c 16.9715(7) _cell_angle_alpha 95.211(3) _cell_angle_beta 91.367(3) _cell_angle_gamma 111.342(3) _cell_volume 2267.24(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5361 _cell_measurement_theta_min 3.0115 _cell_measurement_theta_max 29.1371 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 13.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0830 _exptl_absorpt_correction_T_max 0.1070 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16692 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7999 _reflns_number_gt 5930 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distances of O1W---H1C and O1W---H1D were restrained to 0.87+-0.02 \%A. The distance of H1A...H1B was restrained to 1.44+-0.01 \%A. The distance of H1C...Pb3 was restrained to 2.6+-0.01 \%A. The distance of H15O...O15 was restrained to 0.85+-0.01 \%A. The distances of O15O---Pb2 and O15O---Pb3 were restrained to 2.8+-0.01 \%A. For O1, O2, O3, O14, O2W and O2W', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. For Pb1 and O2, some anisotropic displacement ellipsoids were rather elongated which led us to use the DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7999 _refine_ls_number_parameters 642 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.0000 0.0000 1.0000 0.04190(19) Uani 1 2 d SU . . Pb2 Pb -0.30661(4) 0.05530(4) 0.95355(3) 0.04085(16) Uani 1 1 d D . . Pb3 Pb -0.00486(4) 0.31322(4) 0.97757(3) 0.04792(17) Uani 1 1 d D . . Pb4 Pb 0.10468(5) 0.56813(5) 0.61037(4) 0.0745(2) Uani 1 1 d . . . C1 C -0.0027(13) 0.0935(12) 0.7502(7) 0.052(3) Uani 1 1 d . . . C2 C 0.0371(13) 0.0228(12) 0.7015(8) 0.058(4) Uani 1 1 d . . . H2 H 0.0246 -0.0482 0.7154 0.070 Uiso 1 1 calc R . . C3 C 0.0941(14) 0.0544(12) 0.6338(8) 0.057(4) Uani 1 1 d . . . C4 C 0.1138(12) 0.1600(11) 0.6121(8) 0.053(3) Uani 1 1 d . . . H4 H 0.1548 0.1828 0.5662 0.063 Uiso 1 1 calc R . . C5 C 0.0714(12) 0.2312(11) 0.6600(8) 0.049(3) Uani 1 1 d . . . C6 C 0.0140(12) 0.1962(12) 0.7285(8) 0.054(4) Uani 1 1 d . . . H6 H -0.0141 0.2439 0.7608 0.065 Uiso 1 1 calc R . . C7 C -0.0627(14) 0.0562(13) 0.8282(8) 0.061(4) Uani 1 1 d . . . C8 C 0.0870(13) 0.3432(13) 0.6357(10) 0.060(4) Uani 1 1 d . . . C9 C 0.2379(15) 0.0195(10) 0.5407(9) 0.062(4) Uani 1 1 d . . . H9A H 0.3087 0.0801 0.5697 0.074 Uiso 1 1 calc R . . H9B H 0.2108 0.0472 0.4949 0.074 Uiso 1 1 calc R . . C10 C 0.2797(13) -0.0761(11) 0.5148(8) 0.053(3) Uani 1 1 d . . . C11 C 0.3594(16) -0.1055(13) 0.5649(10) 0.072(5) Uani 1 1 d . . . H11 H 0.3884 -0.0660 0.6146 0.086 Uiso 1 1 calc R . . C12 C 0.3951(15) -0.1947(13) 0.5397(10) 0.074(5) Uani 1 1 d . . . H12 H 0.4502 -0.2137 0.5724 0.089 Uiso 1 1 calc R . . C13 C 0.3492(12) -0.2567(10) 0.4659(9) 0.056(4) Uani 1 1 d . . . C14 C 0.2662(13) -0.2298(10) 0.4195(9) 0.054(4) Uani 1 1 d . . . H14 H 0.2315 -0.2725 0.3715 0.064 Uiso 1 1 calc R . . C15 C 0.2324(12) -0.1366(10) 0.4443(7) 0.046(3) Uani 1 1 d . . . H15 H 0.1775 -0.1172 0.4118 0.055 Uiso 1 1 calc R . . C16 C 0.3906(14) -0.3520(12) 0.4410(12) 0.080(5) Uani 1 1 d . . . C17 C 0.526(3) -0.336(2) 0.4755(19) 0.055(7) Uiso 0.50 1 d P . . C17' C 0.517(3) -0.329(2) 0.4311(18) 0.048(6) Uiso 0.50 1 d P . . C18 C 0.570(3) -0.420(3) 0.446(2) 0.070(9) Uiso 0.50 1 d P . . C18' C 0.574(3) -0.403(3) 0.400(2) 0.061(8) Uiso 0.50 1 d P . . C19 C 0.494(3) -0.515(3) 0.398(2) 0.073(9) Uiso 0.50 1 d P . . C19' C 0.485(3) -0.503(3) 0.351(2) 0.068(8) Uiso 0.50 1 d P . . C20 C 0.363(3) -0.537(3) 0.392(2) 0.075(9) Uiso 0.50 1 d P . . C20' C 0.355(2) -0.525(2) 0.3477(17) 0.045(6) Uiso 0.50 1 d P . . C21 C 0.3094(14) -0.4519(12) 0.4000(12) 0.084(6) Uani 1 1 d . . . C22 C 0.1680(14) -0.4843(12) 0.3908(13) 0.080(6) Uani 1 1 d . . . C23 C -0.3772(10) 0.3537(9) 1.0301(7) 0.034(3) Uani 1 1 d . . . C24 C -0.4937(10) 0.2713(10) 1.0034(7) 0.041(3) Uani 1 1 d . . . H24 H -0.4960 0.2091 0.9703 0.050 Uiso 1 1 calc R . . C25 C -0.6071(10) 0.2821(10) 1.0265(8) 0.044(3) Uani 1 1 d . . . C26 C -0.6048(11) 0.3758(10) 1.0717(7) 0.042(3) Uani 1 1 d . . . H26 H -0.6816 0.3843 1.0842 0.051 Uiso 1 1 calc R . . C27 C -0.4875(11) 0.4584(10) 1.0990(8) 0.046(3) Uani 1 1 d . . . C28 C -0.3743(11) 0.4472(10) 1.0767(7) 0.043(3) Uani 1 1 d . . . H28 H -0.2956 0.5033 1.0934 0.051 Uiso 1 1 calc R . . C29 C -0.2523(11) 0.3442(10) 1.0028(8) 0.045(3) Uani 1 1 d . . . C30 C -0.7359(11) 0.1920(10) 1.0010(7) 0.044(3) Uani 1 1 d . . . C31 C -0.3936(15) 0.6336(13) 1.1748(12) 0.082(5) Uani 1 1 d . . . H31A H -0.3303 0.6532 1.1350 0.098 Uiso 1 1 calc R . . H31B H -0.3553 0.6134 1.2199 0.098 Uiso 1 1 calc R . . C32 C -0.4315(14) 0.7356(13) 1.2009(9) 0.062(4) Uani 1 1 d . . . C33 C -0.5587(16) 0.7189(12) 1.2071(9) 0.070(4) Uani 1 1 d . . . H33 H -0.6206 0.6471 1.2034 0.084 Uiso 1 1 calc R . . C34 C -0.5955(18) 0.8163(13) 1.2197(9) 0.076(5) Uani 1 1 d . . . H34 H -0.6815 0.8081 1.2230 0.091 Uiso 1 1 calc R . . C35 C -0.4985(14) 0.9215(11) 1.2267(7) 0.052(3) Uani 1 1 d . . . C36 C -0.3682(15) 0.9314(12) 1.2222(8) 0.062(4) Uani 1 1 d . . . H36 H -0.3028 1.0016 1.2293 0.074 Uiso 1 1 calc R . . C37 C -0.3373(16) 0.8356(13) 1.2069(10) 0.078(5) Uani 1 1 d . . . H37 H -0.2524 0.8420 1.2010 0.093 Uiso 1 1 calc R . . C38 C -0.5333(10) 1.0228(10) 1.2367(7) 0.037(3) Uani 1 1 d . . . C39 C -0.6294(14) 1.0275(11) 1.2868(8) 0.056(3) Uani 1 1 d . . . H39 H -0.6712 0.9669 1.3145 0.067 Uiso 1 1 calc R . . C40 C -0.6631(14) 1.1198(12) 1.2959(8) 0.061(4) Uani 1 1 d . . . H40 H -0.7288 1.1205 1.3284 0.073 Uiso 1 1 calc R . . C41 C -0.6008(13) 1.2093(12) 1.2577(8) 0.058(4) Uani 1 1 d . . . H41 H -0.6236 1.2718 1.2641 0.069 Uiso 1 1 calc R . . C42 C -0.5040(13) 1.2092(10) 1.2094(7) 0.049(3) Uani 1 1 d . . . H42 H -0.4600 1.2726 1.1849 0.059 Uiso 1 1 calc R . . C43 C -0.4712(11) 1.1159(10) 1.1967(7) 0.039(3) Uani 1 1 d . . . C44 C -0.3731(11) 1.1198(12) 1.1364(7) 0.048(3) Uani 1 1 d . . . O1 O -0.0996(10) 0.1256(10) 0.8669(6) 0.080(3) Uani 1 1 d U . . O2 O -0.0642(9) -0.0324(8) 0.8495(5) 0.0567(12) Uani 1 1 d U . . O3 O 0.0661(13) 0.4109(10) 0.6857(8) 0.097(4) Uani 1 1 d U . . O4 O 0.1165(9) 0.3661(8) 0.5685(7) 0.064(3) Uani 1 1 d . . . O5 O 0.1335(10) -0.0218(8) 0.5902(6) 0.069(3) Uani 1 1 d . . . O6 O 0.1061(8) -0.4641(7) 0.4493(6) 0.061(3) Uani 1 1 d . . . O7 O 0.1053(10) -0.5395(10) 0.3268(8) 0.096(4) Uani 1 1 d . . . O8 O -0.1482(8) 0.4146(8) 1.0351(6) 0.063(3) Uani 1 1 d . . . O9 O -0.2574(8) 0.2642(7) 0.9532(5) 0.055(2) Uani 1 1 d . . . O10 O -0.8335(8) 0.2152(8) 0.9958(7) 0.074(3) Uani 1 1 d . . . O11 O -0.7431(7) 0.0935(7) 0.9879(6) 0.054(2) Uani 1 1 d . . . O12 O -0.4976(10) 0.5475(8) 1.1451(7) 0.081(4) Uani 1 1 d . . . O13 O -0.4180(7) 1.0579(7) 1.0716(5) 0.048(2) Uani 1 1 d . . . O14 O -0.265(2) 1.2017(18) 1.1387(13) 0.041(6) Uani 0.50 1 d PU . . O14' O -0.257(2) 1.163(2) 1.1599(12) 0.043(6) Uani 0.50 1 d P . . O2W O -0.134(3) 1.295(3) 1.2736(18) 0.125(10) Uani 0.50 1 d PU . . O2W' O -0.169(2) 1.3784(18) 1.2296(12) 0.076(6) Uani 0.50 1 d PU . . O3W O 0.0076(17) 0.2653(13) 0.4168(10) 0.151(6) Uani 1 1 d . . . O4W O 0.1036(14) 0.2500(12) 1.2208(7) 0.102(4) Uani 1 1 d . . . O5W O -0.0110(17) 0.5208(18) 1.1682(11) 0.060(6) Uani 0.50 1 d P . . O5W' O 0.075(3) 0.590(2) 1.1707(14) 0.096(8) Uani 0.50 1 d P . . O15 O -0.1134(7) 0.1496(7) 1.0291(5) 0.046(2) Uani 1 1 d D . . H15O H -0.120(2) 0.151(2) 1.0790(7) 0.069 Uiso 1 1 d D . . O1W O 0.0889(10) 0.3861(9) 1.1136(7) 0.076(3) Uani 1 1 d D . . H1C H 0.025(9) 0.334(8) 1.1313(8) 0.114 Uiso 1 1 d D . . H1D H 0.099(15) 0.452(4) 1.136(9) 0.114 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0282(3) 0.0534(4) 0.0445(4) 0.0045(3) 0.0038(3) 0.0155(3) Pb2 0.0271(2) 0.0525(3) 0.0415(3) -0.0093(2) 0.00066(18) 0.0164(2) Pb3 0.0335(3) 0.0480(3) 0.0656(3) 0.0018(3) 0.0080(2) 0.0197(2) Pb4 0.0434(3) 0.0458(3) 0.1275(6) -0.0149(4) 0.0087(3) 0.0139(2) C1 0.054(8) 0.071(10) 0.040(7) 0.012(7) 0.003(6) 0.033(7) C2 0.060(9) 0.061(9) 0.059(9) -0.002(8) 0.009(7) 0.029(7) C3 0.067(9) 0.057(9) 0.062(9) 0.009(8) 0.017(7) 0.038(7) C4 0.043(7) 0.067(9) 0.055(8) -0.001(7) 0.015(6) 0.029(7) C5 0.043(7) 0.057(8) 0.051(8) -0.002(7) 0.002(6) 0.026(6) C6 0.048(8) 0.072(10) 0.049(8) -0.012(7) 0.008(6) 0.035(7) C7 0.067(10) 0.074(10) 0.040(8) -0.006(8) 0.006(7) 0.026(8) C8 0.053(8) 0.071(10) 0.069(10) -0.023(9) -0.002(7) 0.044(8) C9 0.086(11) 0.035(7) 0.071(9) 0.011(7) 0.045(8) 0.026(7) C10 0.051(8) 0.050(8) 0.053(8) -0.002(7) 0.021(7) 0.013(6) C11 0.086(12) 0.059(10) 0.066(10) -0.017(9) -0.013(9) 0.029(9) C12 0.063(10) 0.070(11) 0.080(11) -0.008(10) -0.018(8) 0.019(8) C13 0.038(7) 0.031(7) 0.096(11) -0.006(7) 0.016(7) 0.013(6) C14 0.057(9) 0.036(7) 0.064(9) 0.001(7) 0.023(7) 0.012(6) C15 0.049(7) 0.052(8) 0.042(7) 0.017(7) 0.013(6) 0.023(6) C16 0.042(8) 0.043(8) 0.151(16) -0.006(10) 0.017(9) 0.013(6) C21 0.047(9) 0.037(8) 0.161(18) -0.018(10) 0.018(9) 0.015(7) C22 0.041(8) 0.040(8) 0.147(17) -0.023(10) 0.022(10) 0.007(6) C23 0.024(6) 0.033(6) 0.050(7) 0.013(6) 0.010(5) 0.013(5) C24 0.027(6) 0.048(7) 0.054(7) 0.001(6) 0.002(5) 0.021(5) C25 0.025(6) 0.037(7) 0.072(9) 0.012(6) -0.001(6) 0.014(5) C26 0.040(7) 0.042(7) 0.052(7) 0.005(6) 0.015(6) 0.022(5) C27 0.038(7) 0.034(6) 0.067(9) -0.005(6) 0.004(6) 0.016(5) C28 0.030(6) 0.040(7) 0.057(8) 0.007(6) 0.005(5) 0.010(5) C29 0.027(6) 0.044(7) 0.065(8) 0.001(7) 0.002(6) 0.015(5) C30 0.037(7) 0.041(7) 0.057(8) 0.005(6) 0.020(6) 0.018(5) C31 0.057(10) 0.065(10) 0.126(15) 0.006(11) 0.012(10) 0.026(8) C32 0.048(9) 0.068(10) 0.072(10) 0.018(8) -0.001(7) 0.023(7) C33 0.087(12) 0.046(9) 0.068(10) -0.002(8) 0.012(8) 0.014(8) C34 0.106(14) 0.062(10) 0.063(10) 0.010(9) 0.014(9) 0.035(10) C35 0.076(10) 0.051(8) 0.029(6) -0.012(6) -0.008(6) 0.029(7) C36 0.067(10) 0.063(9) 0.064(9) -0.006(8) -0.007(7) 0.038(8) C37 0.069(11) 0.067(10) 0.107(13) -0.016(10) -0.026(9) 0.044(9) C38 0.035(6) 0.045(7) 0.038(6) 0.000(6) -0.006(5) 0.023(5) C39 0.071(10) 0.049(8) 0.054(8) 0.018(7) 0.018(7) 0.025(7) C40 0.074(10) 0.060(9) 0.057(9) 0.006(8) 0.034(8) 0.033(8) C41 0.056(8) 0.066(9) 0.065(9) -0.004(8) 0.015(7) 0.041(8) C42 0.068(9) 0.036(7) 0.043(7) 0.002(6) 0.007(6) 0.018(6) C43 0.041(7) 0.045(7) 0.033(6) -0.014(6) 0.000(5) 0.022(6) C44 0.035(7) 0.066(9) 0.044(7) -0.010(7) 0.007(6) 0.021(6) O1 0.072(6) 0.090(7) 0.062(6) -0.005(5) 0.023(5) 0.013(5) O2 0.0587(16) 0.0585(16) 0.0515(11) 0.0072(10) 0.0013(10) 0.0197(10) O3 0.119(8) 0.088(7) 0.104(7) 0.003(6) 0.013(6) 0.063(6) O4 0.057(6) 0.061(6) 0.082(7) 0.006(6) 0.022(5) 0.030(5) O5 0.085(7) 0.053(6) 0.080(7) 0.014(5) 0.046(6) 0.034(5) O6 0.048(5) 0.038(5) 0.095(7) 0.009(5) 0.026(5) 0.013(4) O7 0.056(7) 0.086(8) 0.130(10) -0.035(8) 0.017(7) 0.019(6) O8 0.034(5) 0.066(6) 0.082(7) -0.018(5) -0.004(4) 0.016(4) O9 0.036(5) 0.057(6) 0.075(6) -0.007(5) 0.011(4) 0.024(4) O10 0.028(5) 0.057(6) 0.136(10) 0.000(6) -0.004(5) 0.018(4) O11 0.025(4) 0.054(6) 0.083(7) -0.003(5) 0.005(4) 0.018(4) O12 0.063(7) 0.041(6) 0.138(10) -0.028(6) -0.005(6) 0.027(5) O13 0.034(4) 0.065(6) 0.040(5) -0.015(5) 0.007(4) 0.018(4) O14 0.042(9) 0.037(9) 0.039(10) -0.008(7) 0.001(7) 0.013(7) O14' 0.026(10) 0.063(15) 0.033(11) 0.016(10) 0.004(8) 0.007(10) O2W 0.114(12) 0.129(13) 0.117(12) -0.016(9) 0.005(9) 0.036(9) O2W' 0.077(9) 0.077(9) 0.056(9) -0.003(8) 0.012(7) 0.008(7) O3W 0.172(16) 0.099(11) 0.144(14) 0.041(11) 0.006(11) -0.002(10) O4W 0.128(11) 0.116(11) 0.082(8) 0.016(8) 0.021(8) 0.066(9) O5W 0.040(11) 0.062(13) 0.044(11) -0.019(10) 0.011(8) -0.015(9) O5W' 0.16(3) 0.073(17) 0.065(15) -0.015(14) 0.026(17) 0.054(18) O15 0.028(4) 0.061(5) 0.044(5) -0.011(4) -0.001(3) 0.015(4) O1W 0.071(7) 0.068(7) 0.091(8) -0.018(6) -0.014(6) 0.036(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O2 2.591(9) 2_557 ? Pb1 O2 2.591(9) . ? Pb1 O15 2.688(8) . ? Pb1 O15 2.688(8) 2_557 ? Pb1 O11 2.697(8) 2_457 ? Pb1 O11 2.697(8) 1_655 ? Pb1 O10 2.735(10) 2_457 ? Pb1 O10 2.735(10) 1_655 ? Pb2 O15 2.335(7) . ? Pb2 O13 2.387(7) 1_545 ? Pb2 O11 2.468(9) 2_457 ? Pb2 O9 2.554(9) . ? Pb2 O1 2.684(10) . ? Pb3 O15 2.287(9) . ? Pb3 O1W 2.466(10) . ? Pb3 O8 2.569(8) . ? Pb3 O9 2.667(8) . ? Pb3 O10 2.677(9) 1_655 ? Pb4 O6 2.388(9) 2_556 ? Pb4 O3 2.412(13) . ? Pb4 O2W 2.45(3) 2_577 ? Pb4 O7 2.515(10) 2_556 ? Pb4 O4 2.695(9) . ? Pb4 O6 2.729(10) 1_565 ? Pb4 O2W' 2.75(2) 2_577 ? Pb4 C22 2.833(14) 2_556 ? C1 C6 1.36(2) . ? C1 C2 1.377(17) . ? C1 C7 1.535(19) . ? C2 C3 1.349(19) . ? C2 H2 0.9300 . ? C3 O5 1.383(14) . ? C3 C4 1.387(19) . ? C4 C5 1.389(15) . ? C4 H4 0.9300 . ? C5 C6 1.374(19) . ? C5 C8 1.49(2) . ? C6 H6 0.9300 . ? C7 O2 1.226(17) . ? C7 O1 1.257(16) . ? C8 O4 1.226(18) . ? C8 O3 1.250(15) . ? C9 O5 1.422(15) . ? C9 C10 1.507(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.350(17) . ? C10 C11 1.39(2) . ? C11 C12 1.39(2) . ? C11 H11 0.9300 . ? C12 C13 1.40(2) . ? C12 H12 0.9300 . ? C13 C14 1.360(19) . ? C13 C16 1.496(17) . ? C14 C15 1.420(16) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17' 1.35(3) . ? C16 C21 1.39(2) . ? C16 C17 1.54(3) . ? C17 C17' 0.77(3) . ? C17 C18 1.41(4) . ? C17 C18' 1.70(4) . ? C17' C18' 1.40(4) . ? C17' C18 1.53(4) . ? C18 C18' 0.83(4) . ? C18 C19 1.39(4) . ? C18 C19' 1.89(5) . ? C18' C19 1.39(4) . ? C18' C19' 1.48(4) . ? C19 C19' 0.84(4) . ? C19 C20 1.38(4) . ? C19 C20' 1.71(4) . ? C19' C20' 1.38(4) . ? C19' C20 1.49(5) . ? C20 C20' 0.79(4) . ? C20 C21 1.43(4) . ? C20' C21 1.47(3) . ? C21 C22 1.48(2) . ? C22 O7 1.28(2) . ? C22 O6 1.283(18) . ? C22 Pb4 2.833(14) 2_556 ? C23 C28 1.374(15) . ? C23 C24 1.381(15) . ? C23 C29 1.522(14) . ? C24 C25 1.385(15) . ? C24 H24 0.9300 . ? C25 C26 1.365(15) . ? C25 C30 1.506(16) . ? C26 C27 1.391(16) . ? C26 H26 0.9300 . ? C27 O12 1.373(13) . ? C27 C28 1.380(15) . ? C28 H28 0.9300 . ? C29 O9 1.256(13) . ? C29 O8 1.260(14) . ? C30 O10 1.234(13) . ? C30 O11 1.246(13) . ? C31 O12 1.331(17) . ? C31 C32 1.56(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C37 1.33(2) . ? C32 C33 1.364(19) . ? C33 C34 1.46(2) . ? C33 H33 0.9300 . ? C34 C35 1.39(2) . ? C34 H34 0.9300 . ? C35 C36 1.418(18) . ? C35 C38 1.493(16) . ? C36 C37 1.406(18) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.399(17) . ? C38 C43 1.398(17) . ? C39 C40 1.373(18) . ? C39 H39 0.9300 . ? C40 C41 1.35(2) . ? C40 H40 0.9300 . ? C41 C42 1.371(17) . ? C41 H41 0.9300 . ? C42 C43 1.383(16) . ? C42 H42 0.9300 . ? C43 C44 1.506(16) . ? C44 O14' 1.25(2) . ? C44 O13 1.275(14) . ? C44 O14 1.28(3) . ? O6 Pb4 2.388(9) 2_556 ? O6 Pb4 2.729(10) 1_545 ? O7 Pb4 2.515(10) 2_556 ? O10 Pb3 2.677(9) 1_455 ? O10 Pb1 2.735(10) 1_455 ? O11 Pb2 2.468(9) 2_457 ? O11 Pb1 2.697(8) 1_455 ? O13 Pb2 2.387(7) 1_565 ? O14 O14' 0.68(2) . ? O2W O2W' 1.52(4) . ? O2W Pb4 2.45(3) 2_577 ? O2W' Pb4 2.75(2) 2_577 ? O5W O5W' 1.04(3) . ? O15 H15O 0.850(10) . ? O1W H1C 0.87(2) . ? O1W H1D 0.87(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Pb1 O2 180.000(2) 2_557 . ? O2 Pb1 O15 86.3(3) 2_557 . ? O2 Pb1 O15 93.7(3) . . ? O2 Pb1 O15 93.7(3) 2_557 2_557 ? O2 Pb1 O15 86.3(3) . 2_557 ? O15 Pb1 O15 180.000(2) . 2_557 ? O2 Pb1 O11 96.9(3) 2_557 2_457 ? O2 Pb1 O11 83.1(3) . 2_457 ? O15 Pb1 O11 66.3(2) . 2_457 ? O15 Pb1 O11 113.7(2) 2_557 2_457 ? O2 Pb1 O11 83.1(3) 2_557 1_655 ? O2 Pb1 O11 96.9(3) . 1_655 ? O15 Pb1 O11 113.7(2) . 1_655 ? O15 Pb1 O11 66.3(2) 2_557 1_655 ? O11 Pb1 O11 180.0(4) 2_457 1_655 ? O2 Pb1 O10 94.5(3) 2_557 2_457 ? O2 Pb1 O10 85.5(3) . 2_457 ? O15 Pb1 O10 112.7(3) . 2_457 ? O15 Pb1 O10 67.3(3) 2_557 2_457 ? O11 Pb1 O10 46.7(3) 2_457 2_457 ? O11 Pb1 O10 133.3(3) 1_655 2_457 ? O2 Pb1 O10 85.5(3) 2_557 1_655 ? O2 Pb1 O10 94.5(3) . 1_655 ? O15 Pb1 O10 67.3(3) . 1_655 ? O15 Pb1 O10 112.7(3) 2_557 1_655 ? O11 Pb1 O10 133.3(3) 2_457 1_655 ? O11 Pb1 O10 46.7(3) 1_655 1_655 ? O10 Pb1 O10 180.0(5) 2_457 1_655 ? O15 Pb2 O13 88.3(3) . 1_545 ? O15 Pb2 O11 75.6(3) . 2_457 ? O13 Pb2 O11 83.1(3) 1_545 2_457 ? O15 Pb2 O9 72.7(3) . . ? O13 Pb2 O9 89.1(3) 1_545 . ? O11 Pb2 O9 147.5(3) 2_457 . ? O15 Pb2 O1 66.2(3) . . ? O13 Pb2 O1 153.2(3) 1_545 . ? O11 Pb2 O1 97.5(3) 2_457 . ? O9 Pb2 O1 76.0(3) . . ? O15 Pb3 O1W 86.0(3) . . ? O15 Pb3 O8 94.8(3) . . ? O1W Pb3 O8 75.7(3) . . ? O15 Pb3 O9 71.2(3) . . ? O1W Pb3 O9 116.8(3) . . ? O8 Pb3 O9 50.0(2) . . ? O15 Pb3 O10 74.1(3) . 1_655 ? O1W Pb3 O10 77.1(3) . 1_655 ? O8 Pb3 O10 151.2(3) . 1_655 ? O9 Pb3 O10 141.2(3) . 1_655 ? O6 Pb4 O3 84.7(4) 2_556 . ? O6 Pb4 O2W 120.2(7) 2_556 2_577 ? O3 Pb4 O2W 95.0(9) . 2_577 ? O6 Pb4 O7 53.6(3) 2_556 2_556 ? O3 Pb4 O7 74.1(4) . 2_556 ? O2W Pb4 O7 68.9(7) 2_577 2_556 ? O6 Pb4 O4 77.6(3) 2_556 . ? O3 Pb4 O4 49.8(3) . . ? O2W Pb4 O4 141.2(9) 2_577 . ? O7 Pb4 O4 108.2(4) 2_556 . ? O6 Pb4 O6 68.2(3) 2_556 1_565 ? O3 Pb4 O6 119.0(3) . 1_565 ? O2W Pb4 O6 145.9(8) 2_577 1_565 ? O7 Pb4 O6 119.3(4) 2_556 1_565 ? O4 Pb4 O6 70.9(3) . 1_565 ? O6 Pb4 O2W' 126.0(5) 2_556 2_577 ? O3 Pb4 O2W' 64.8(6) . 2_577 ? O2W Pb4 O2W' 33.2(8) 2_577 2_577 ? O7 Pb4 O2W' 74.9(5) 2_556 2_577 ? O4 Pb4 O2W' 108.0(6) . 2_577 ? O6 Pb4 O2W' 165.6(5) 1_565 2_577 ? O6 Pb4 C22 26.7(4) 2_556 2_556 ? O3 Pb4 C22 79.2(5) . 2_556 ? O2W Pb4 C22 94.4(8) 2_577 2_556 ? O7 Pb4 C22 26.9(4) 2_556 2_556 ? O4 Pb4 C22 93.9(3) . 2_556 ? O6 Pb4 C22 93.5(5) 1_565 2_556 ? O2W' Pb4 C22 100.9(6) 2_577 2_556 ? C6 C1 C2 118.8(12) . . ? C6 C1 C7 121.3(12) . . ? C2 C1 C7 119.8(13) . . ? C3 C2 C1 121.3(14) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 O5 116.7(13) . . ? C2 C3 C4 120.1(12) . . ? O5 C3 C4 123.2(12) . . ? C3 C4 C5 119.1(13) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 119.2(13) . . ? C6 C5 C8 121.1(11) . . ? C4 C5 C8 119.7(12) . . ? C1 C6 C5 121.4(11) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? O2 C7 O1 126.1(13) . . ? O2 C7 C1 119.2(12) . . ? O1 C7 C1 114.6(14) . . ? O4 C8 O3 122.0(16) . . ? O4 C8 C5 120.6(11) . . ? O3 C8 C5 117.4(15) . . ? O5 C9 C10 107.3(10) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? C15 C10 C11 120.6(12) . . ? C15 C10 C9 119.0(14) . . ? C11 C10 C9 120.3(13) . . ? C12 C11 C10 118.9(13) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 121.1(15) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 118.9(12) . . ? C14 C13 C16 121.8(14) . . ? C12 C13 C16 119.2(15) . . ? C13 C14 C15 120.0(12) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 120.3(13) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17' C16 C21 113.9(15) . . ? C17' C16 C13 118.2(16) . . ? C21 C16 C13 123.6(13) . . ? C17' C16 C17 30.2(14) . . ? C21 C16 C17 122.5(15) . . ? C13 C16 C17 113.3(15) . . ? C17' C17 C18 84(4) . . ? C17' C17 C16 61(3) . . ? C18 C17 C16 113(2) . . ? C17' C17 C18' 55(3) . . ? C18 C17 C18' 29.3(16) . . ? C16 C17 C18' 99(2) . . ? C17 C17' C16 88(3) . . ? C17 C17' C18' 98(4) . . ? C16 C17' C18' 127(2) . . ? C17 C17' C18 66(3) . . ? C16 C17' C18 117(2) . . ? C18' C17' C18 32.7(16) . . ? C18' C18 C19 72(4) . . ? C18' C18 C17 95(4) . . ? C19 C18 C17 123(3) . . ? C18' C18 C17' 65(3) . . ? C19 C18 C17' 106(3) . . ? C17 C18 C17' 30.2(15) . . ? C18' C18 C19' 49(3) . . ? C19 C18 C19' 24.1(19) . . ? C17 C18 C19' 115(3) . . ? C17' C18 C19' 90(2) . . ? C18 C18' C19 73(4) . . ? C18 C18' C17' 82(4) . . ? C19 C18' C17' 113(3) . . ? C18 C18' C19' 106(4) . . ? C19 C18' C19' 34.1(18) . . ? C17' C18' C19' 115(3) . . ? C18 C18' C17 56(3) . . ? C19 C18' C17 105(3) . . ? C17' C18' C17 26.8(14) . . ? C19' C18' C17 123(3) . . ? C19' C19 C20 80(4) . . ? C19' C19 C18 114(5) . . ? C20 C19 C18 117(3) . . ? C19' C19 C18' 79(4) . . ? C20 C19 C18' 116(3) . . ? C18 C19 C18' 35.0(18) . . ? C19' C19 C20' 53(3) . . ? C20 C19 C20' 27.0(17) . . ? C18 C19 C20' 123(3) . . ? C18' C19 C20' 105(3) . . ? C19 C19' C20' 98(4) . . ? C19 C19' C18' 67(4) . . ? C20' C19' C18' 120(3) . . ? C19 C19' C20 66(4) . . ? C20' C19' C20 31.6(16) . . ? C18' C19' C20 105(3) . . ? C19 C19' C18 42(3) . . ? C20' C19' C18 112(2) . . ? C18' C19' C18 25.1(16) . . ? C20 C19' C18 88(2) . . ? C20' C20 C19 100(4) . . ? C20' C20 C21 77(4) . . ? C19 C20 C21 123(3) . . ? C20' C20 C19' 66(4) . . ? C19 C20 C19' 33.8(18) . . ? C21 C20 C19' 113(3) . . ? C20 C20' C19' 82(4) . . ? C20 C20' C21 71(3) . . ? C19' C20' C21 117(2) . . ? C20 C20' C19 53(3) . . ? C19' C20' C19 29.2(17) . . ? C21 C20' C19 102(2) . . ? C16 C21 C20 114.4(19) . . ? C16 C21 C20' 123.8(15) . . ? C20 C21 C20' 31.5(15) . . ? C16 C21 C22 123.2(12) . . ? C20 C21 C22 118.9(18) . . ? C20' C21 C22 111.8(15) . . ? O7 C22 O6 119.4(13) . . ? O7 C22 C21 120.5(14) . . ? O6 C22 C21 119.9(17) . . ? O7 C22 Pb4 62.6(7) . 2_556 ? O6 C22 Pb4 56.9(7) . 2_556 ? C21 C22 Pb4 171.7(14) . 2_556 ? C28 C23 C24 120.1(10) . . ? C28 C23 C29 120.1(10) . . ? C24 C23 C29 119.6(10) . . ? C23 C24 C25 119.3(10) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.7(11) . . ? C26 C25 C30 118.5(10) . . ? C24 C25 C30 120.8(11) . . ? C25 C26 C27 119.9(10) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? O12 C27 C28 126.0(11) . . ? O12 C27 C26 114.6(10) . . ? C28 C27 C26 119.4(10) . . ? C23 C28 C27 120.4(10) . . ? C23 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? O9 C29 O8 123.2(10) . . ? O9 C29 C23 119.3(10) . . ? O8 C29 C23 117.4(10) . . ? O10 C30 O11 120.5(11) . . ? O10 C30 C25 120.3(10) . . ? O11 C30 C25 119.1(10) . . ? O12 C31 C32 109.9(12) . . ? O12 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O12 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C37 C32 C33 124.2(14) . . ? C37 C32 C31 116.5(13) . . ? C33 C32 C31 118.8(13) . . ? C32 C33 C34 118.6(14) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C35 C34 C33 118.1(16) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 119.7(13) . . ? C34 C35 C38 119.5(13) . . ? C36 C35 C38 120.8(12) . . ? C37 C36 C35 120.3(14) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C32 C37 C36 119.0(15) . . ? C32 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C39 C38 C43 117.8(10) . . ? C39 C38 C35 120.8(12) . . ? C43 C38 C35 121.4(11) . . ? C40 C39 C38 121.4(13) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C41 C40 C39 119.8(12) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.7(12) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C43 120.8(13) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C42 C43 C38 119.4(10) . . ? C42 C43 C44 116.8(12) . . ? C38 C43 C44 123.8(10) . . ? O14' C44 O13 125.6(14) . . ? O14' C44 O14 30.9(11) . . ? O13 C44 O14 119.7(15) . . ? O14' C44 C43 117.5(14) . . ? O13 C44 C43 115.0(10) . . ? O14 C44 C43 121.9(15) . . ? C7 O1 Pb2 120.3(10) . . ? C7 O2 Pb1 107.9(8) . . ? C8 O3 Pb4 100.6(11) . . ? C8 O4 Pb4 87.6(8) . . ? C3 O5 C9 118.3(10) . . ? C22 O6 Pb4 96.4(9) . 2_556 ? C22 O6 Pb4 145.4(11) . 1_545 ? Pb4 O6 Pb4 111.8(3) 2_556 1_545 ? C22 O7 Pb4 90.5(8) . 2_556 ? C29 O8 Pb3 95.4(7) . . ? C29 O9 Pb2 136.8(9) . . ? C29 O9 Pb3 90.9(6) . . ? Pb2 O9 Pb3 92.1(3) . . ? C30 O10 Pb3 166.2(9) . 1_455 ? C30 O10 Pb1 94.4(8) . 1_455 ? Pb3 O10 Pb1 99.2(3) 1_455 1_455 ? C30 O11 Pb2 143.3(9) . 2_457 ? C30 O11 Pb1 95.9(7) . 1_455 ? Pb2 O11 Pb1 95.3(3) 2_457 1_455 ? C31 O12 C27 121.5(11) . . ? C44 O13 Pb2 126.9(8) . 1_565 ? O14' O14 C44 72(3) . . ? O14 O14' C44 77(3) . . ? O2W' O2W Pb4 84.4(14) . 2_577 ? O2W O2W' Pb4 62.4(12) . 2_577 ? Pb3 O15 Pb2 108.9(4) . . ? Pb3 O15 Pb1 111.6(3) . . ? Pb2 O15 Pb1 98.8(3) . . ? Pb3 O15 H15O 118.8(15) . . ? Pb2 O15 H15O 114.7(13) . . ? Pb1 O15 H15O 102(3) . . ? Pb3 O1W H1C 89.0(11) . . ? Pb3 O1W H1D 124(10) . . ? H1C O1W H1D 113(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1(2) . . . . ? C7 C1 C2 C3 -177.8(14) . . . . ? C1 C2 C3 O5 178.4(12) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? O5 C3 C4 C5 -179.6(12) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C3 C4 C5 C8 -177.4(13) . . . . ? C2 C1 C6 C5 -1(2) . . . . ? C7 C1 C6 C5 177.9(12) . . . . ? C4 C5 C6 C1 0(2) . . . . ? C8 C5 C6 C1 178.7(12) . . . . ? C6 C1 C7 O2 -172.7(13) . . . . ? C2 C1 C7 O2 6(2) . . . . ? C6 C1 C7 O1 3(2) . . . . ? C2 C1 C7 O1 -177.8(13) . . . . ? C6 C5 C8 O4 -166.8(13) . . . . ? C4 C5 C8 O4 12(2) . . . . ? C6 C5 C8 O3 12(2) . . . . ? C4 C5 C8 O3 -169.3(13) . . . . ? O5 C9 C10 C15 95.5(15) . . . . ? O5 C9 C10 C11 -80.7(17) . . . . ? C15 C10 C11 C12 3(2) . . . . ? C9 C10 C11 C12 179.3(14) . . . . ? C10 C11 C12 C13 -2(2) . . . . ? C11 C12 C13 C14 -2(2) . . . . ? C11 C12 C13 C16 179.8(15) . . . . ? C12 C13 C14 C15 3(2) . . . . ? C16 C13 C14 C15 -178.1(12) . . . . ? C11 C10 C15 C14 -2(2) . . . . ? C9 C10 C15 C14 -177.7(11) . . . . ? C13 C14 C15 C10 -1.8(19) . . . . ? C14 C13 C16 C17' 118(2) . . . . ? C12 C13 C16 C17' -63(3) . . . . ? C14 C13 C16 C21 -37(3) . . . . ? C12 C13 C16 C21 141.4(19) . . . . ? C14 C13 C16 C17 151.3(19) . . . . ? C12 C13 C16 C17 -30(2) . . . . ? C21 C16 C17 C17' 82(4) . . . . ? C13 C16 C17 C17' -106(4) . . . . ? C17' C16 C17 C18 -68(4) . . . . ? C21 C16 C17 C18 14(4) . . . . ? C13 C16 C17 C18 -174(2) . . . . ? C17' C16 C17 C18' -41(3) . . . . ? C21 C16 C17 C18' 41(3) . . . . ? C13 C16 C17 C18' -147.5(19) . . . . ? C18 C17 C17' C16 121(2) . . . . ? C18' C17 C17' C16 128(3) . . . . ? C18 C17 C17' C18' -6(3) . . . . ? C16 C17 C17' C18' -128(3) . . . . ? C16 C17 C17' C18 -121(2) . . . . ? C18' C17 C17' C18 6(3) . . . . ? C21 C16 C17' C17 -114(4) . . . . ? C13 C16 C17' C17 88(4) . . . . ? C21 C16 C17' C18' -15(4) . . . . ? C13 C16 C17' C18' -172(3) . . . . ? C17 C16 C17' C18' 99(5) . . . . ? C21 C16 C17' C18 -52(3) . . . . ? C13 C16 C17' C18 150(2) . . . . ? C17 C16 C17' C18 62(4) . . . . ? C17' C17 C18 C18' 11(5) . . . . ? C16 C17 C18 C18' 66(4) . . . . ? C17' C17 C18 C19 -61(5) . . . . ? C16 C17 C18 C19 -6(5) . . . . ? C18' C17 C18 C19 -72(4) . . . . ? C16 C17 C18 C17' 55(3) . . . . ? C18' C17 C18 C17' -11(5) . . . . ? C17' C17 C18 C19' -35(4) . . . . ? C16 C17 C18 C19' 20(4) . . . . ? C18' C17 C18 C19' -46(3) . . . . ? C17 C17' C18 C18' -168(5) . . . . ? C16 C17' C18 C18' 117(4) . . . . ? C17 C17' C18 C19 130(4) . . . . ? C16 C17' C18 C19 56(4) . . . . ? C18' C17' C18 C19 -62(4) . . . . ? C16 C17' C18 C17 -75(4) . . . . ? C18' C17' C18 C17 168(5) . . . . ? C17 C17' C18 C19' 148(4) . . . . ? C16 C17' C18 C19' 74(3) . . . . ? C18' C17' C18 C19' -43(3) . . . . ? C17 C18 C18' C19 -124(3) . . . . ? C17' C18 C18' C19 -118(2) . . . . ? C19' C18 C18' C19 -4(3) . . . . ? C19 C18 C18' C17' 118(2) . . . . ? C17 C18 C18' C17' -6(3) . . . . ? C19' C18 C18' C17' 114(3) . . . . ? C19 C18 C18' C19' 4(3) . . . . ? C17 C18 C18' C19' -119(3) . . . . ? C17' C18 C18' C19' -114(3) . . . . ? C19 C18 C18' C17 124(3) . . . . ? C17' C18 C18' C17 6(3) . . . . ? C19' C18 C18' C17 119(3) . . . . ? C17 C17' C18' C18 11(5) . . . . ? C16 C17' C18' C18 -83(5) . . . . ? C17 C17' C18' C19 78(5) . . . . ? C16 C17' C18' C19 -16(5) . . . . ? C18 C17' C18' C19 67(4) . . . . ? C17 C17' C18' C19' 115(4) . . . . ? C16 C17' C18' C19' 21(5) . . . . ? C18 C17' C18' C19' 104(5) . . . . ? C16 C17' C18' C17 -94(5) . . . . ? C18 C17' C18' C17 -11(5) . . . . ? C17' C17 C18' C18 -167(6) . . . . ? C16 C17 C18' C18 -122(4) . . . . ? C17' C17 C18' C19 -111(4) . . . . ? C18 C17 C18' C19 56(4) . . . . ? C16 C17 C18' C19 -66(3) . . . . ? C18 C17 C18' C17' 167(6) . . . . ? C16 C17 C18' C17' 45(3) . . . . ? C17' C17 C18' C19' -79(5) . . . . ? C18 C17 C18' C19' 88(5) . . . . ? C16 C17 C18' C19' -34(4) . . . . ? C18' C18 C19 C19' -7(5) . . . . ? C17 C18 C19 C19' 77(6) . . . . ? C17' C18 C19 C19' 50(5) . . . . ? C18' C18 C19 C20 -98(5) . . . . ? C17 C18 C19 C20 -14(6) . . . . ? C17' C18 C19 C20 -41(5) . . . . ? C19' C18 C19 C20 -91(5) . . . . ? C17 C18 C19 C18' 84(5) . . . . ? C17' C18 C19 C18' 57(3) . . . . ? C19' C18 C19 C18' 7(5) . . . . ? C18' C18 C19 C20' -68(4) . . . . ? C17 C18 C19 C20' 17(6) . . . . ? C17' C18 C19 C20' -11(5) . . . . ? C19' C18 C19 C20' -60(4) . . . . ? C18 C18' C19 C19' 173(5) . . . . ? C17' C18' C19 C19' 100(4) . . . . ? C17 C18' C19 C19' 127(4) . . . . ? C18 C18' C19 C20 100(4) . . . . ? C17' C18' C19 C20 27(5) . . . . ? C19' C18' C19 C20 -73(4) . . . . ? C17 C18' C19 C20 55(4) . . . . ? C17' C18' C19 C18 -73(4) . . . . ? C19' C18' C19 C18 -173(5) . . . . ? C17 C18' C19 C18 -46(3) . . . . ? C18 C18' C19 C20' 127(4) . . . . ? C17' C18' C19 C20' 54(4) . . . . ? C19' C18' C19 C20' -46(3) . . . . ? C17 C18' C19 C20' 81(3) . . . . ? C20 C19 C19' C20' 1(3) . . . . ? C18 C19 C19' C20' -115(3) . . . . ? C18' C19 C19' C20' -119(3) . . . . ? C20 C19 C19' C18' 120(2) . . . . ? C18 C19 C19' C18' 4(3) . . . . ? C20' C19 C19' C18' 119(3) . . . . ? C18 C19 C19' C20 -115(4) . . . . ? C18' C19 C19' C20 -120(2) . . . . ? C20' C19 C19' C20 -1(3) . . . . ? C20 C19 C19' C18 115(4) . . . . ? C18' C19 C19' C18 -4(3) . . . . ? C20' C19 C19' C18 115(3) . . . . ? C18 C18' C19' C19 -7(5) . . . . ? C17' C18' C19' C19 -95(4) . . . . ? C17 C18' C19' C19 -66(5) . . . . ? C18 C18' C19' C20' 79(5) . . . . ? C19 C18' C19' C20' 86(4) . . . . ? C17' C18' C19' C20' -10(5) . . . . ? C17 C18' C19' C20' 20(5) . . . . ? C18 C18' C19' C20 48(5) . . . . ? C19 C18' C19' C20 55(3) . . . . ? C17' C18' C19' C20 -40(4) . . . . ? C17 C18' C19' C20 -11(4) . . . . ? C19 C18' C19' C18 7(5) . . . . ? C17' C18' C19' C18 -88(4) . . . . ? C17 C18' C19' C18 -59(4) . . . . ? C18' C18 C19' C19 171(7) . . . . ? C17 C18 C19' C19 -116(5) . . . . ? C17' C18 C19' C19 -133(5) . . . . ? C18' C18 C19' C20' -113(5) . . . . ? C19 C18 C19' C20' 76(5) . . . . ? C17 C18 C19' C20' -40(4) . . . . ? C17' C18 C19' C20' -57(3) . . . . ? C19 C18 C19' C18' -171(7) . . . . ? C17 C18 C19' C18' 73(4) . . . . ? C17' C18 C19' C18' 56(4) . . . . ? C18' C18 C19' C20 -134(4) . . . . ? C19 C18 C19' C20 56(4) . . . . ? C17 C18 C19' C20 -60(3) . . . . ? C17' C18 C19' C20 -77(3) . . . . ? C19' C19 C20 C20' -1(5) . . . . ? C18 C19 C20 C20' 111(5) . . . . ? C18' C19 C20 C20' 71(5) . . . . ? C19' C19 C20 C21 -82(5) . . . . ? C18 C19 C20 C21 29(6) . . . . ? C18' C19 C20 C21 -10(6) . . . . ? C20' C19 C20 C21 -81(5) . . . . ? C18 C19 C20 C19' 111(5) . . . . ? C18' C19 C20 C19' 72(4) . . . . ? C20' C19 C20 C19' 1(5) . . . . ? C19 C19' C20 C20' 179(5) . . . . ? C18' C19' C20 C20' 123(4) . . . . ? C18 C19' C20 C20' 141(4) . . . . ? C20' C19' C20 C19 -179(5) . . . . ? C18' C19' C20 C19 -56(4) . . . . ? C18 C19' C20 C19 -38(3) . . . . ? C19 C19' C20 C21 116(4) . . . . ? C20' C19' C20 C21 -63(4) . . . . ? C18' C19' C20 C21 60(4) . . . . ? C18 C19' C20 C21 78(3) . . . . ? C19 C20 C20' C19' 1(3) . . . . ? C21 C20 C20' C19' 122(2) . . . . ? C19 C20 C20' C21 -122(3) . . . . ? C19' C20 C20' C21 -122(2) . . . . ? C21 C20 C20' C19 122(3) . . . . ? C19' C20 C20' C19 -1(3) . . . . ? C19 C19' C20' C20 -1(5) . . . . ? C18' C19' C20' C20 -69(5) . . . . ? C18 C19' C20' C20 -42(4) . . . . ? C19 C19' C20' C21 63(5) . . . . ? C18' C19' C20' C21 -5(5) . . . . ? C20 C19' C20' C21 64(4) . . . . ? C18 C19' C20' C21 22(4) . . . . ? C18' C19' C20' C19 -68(4) . . . . ? C20 C19' C20' C19 1(5) . . . . ? C18 C19' C20' C19 -41(3) . . . . ? C19' C19 C20' C20 179(6) . . . . ? C18 C19 C20' C20 -85(5) . . . . ? C18' C19 C20' C20 -118(5) . . . . ? C20 C19 C20' C19' -179(6) . . . . ? C18 C19 C20' C19' 96(5) . . . . ? C18' C19 C20' C19' 63(4) . . . . ? C19' C19 C20' C21 -126(4) . . . . ? C20 C19 C20' C21 55(4) . . . . ? C18 C19 C20' C21 -30(4) . . . . ? C18' C19 C20' C21 -63(3) . . . . ? C17' C16 C21 C20 32(3) . . . . ? C13 C16 C21 C20 -172(2) . . . . ? C17 C16 C21 C20 -1(3) . . . . ? C17' C16 C21 C20' -2(3) . . . . ? C13 C16 C21 C20' 154(2) . . . . ? C17 C16 C21 C20' -35(3) . . . . ? C17' C16 C21 C22 -169(2) . . . . ? C13 C16 C21 C22 -13(3) . . . . ? C17 C16 C21 C22 158(2) . . . . ? C20' C20 C21 C16 -115(4) . . . . ? C19 C20 C21 C16 -22(5) . . . . ? C19' C20 C21 C16 -58(4) . . . . ? C19 C20 C21 C20' 94(5) . . . . ? C19' C20 C21 C20' 57(3) . . . . ? C20' C20 C21 C22 85(4) . . . . ? C19 C20 C21 C22 179(3) . . . . ? C19' C20 C21 C22 142(3) . . . . ? C20 C20' C21 C16 82(4) . . . . ? C19' C20' C21 C16 12(4) . . . . ? C19 C20' C21 C16 38(3) . . . . ? C19' C20' C21 C20 -70(4) . . . . ? C19 C20' C21 C20 -44(3) . . . . ? C20 C20' C21 C22 -110(4) . . . . ? C19' C20' C21 C22 180(3) . . . . ? C19 C20' C21 C22 -154(2) . . . . ? C16 C21 C22 O7 145(2) . . . . ? C20 C21 C22 O7 -58(3) . . . . ? C20' C21 C22 O7 -24(3) . . . . ? C16 C21 C22 O6 -40(3) . . . . ? C20 C21 C22 O6 117(2) . . . . ? C20' C21 C22 O6 151.5(18) . . . . ? C16 C21 C22 Pb4 -106(7) . . . 2_556 ? C20 C21 C22 Pb4 52(9) . . . 2_556 ? C20' C21 C22 Pb4 86(8) . . . 2_556 ? C28 C23 C24 C25 -2.3(19) . . . . ? C29 C23 C24 C25 -178.0(11) . . . . ? C23 C24 C25 C26 3.4(19) . . . . ? C23 C24 C25 C30 -177.8(12) . . . . ? C24 C25 C26 C27 -4(2) . . . . ? C30 C25 C26 C27 177.3(12) . . . . ? C25 C26 C27 O12 -178.8(12) . . . . ? C25 C26 C27 C28 3(2) . . . . ? C24 C23 C28 C27 1.7(19) . . . . ? C29 C23 C28 C27 177.4(12) . . . . ? O12 C27 C28 C23 -179.9(13) . . . . ? C26 C27 C28 C23 -2(2) . . . . ? C28 C23 C29 O9 -172.2(12) . . . . ? C24 C23 C29 O9 3.6(18) . . . . ? C28 C23 C29 O8 11.7(18) . . . . ? C24 C23 C29 O8 -172.5(13) . . . . ? C26 C25 C30 O10 25.0(19) . . . . ? C24 C25 C30 O10 -153.8(13) . . . . ? C26 C25 C30 O11 -152.5(12) . . . . ? C24 C25 C30 O11 28.7(19) . . . . ? O12 C31 C32 C37 -158.5(16) . . . . ? O12 C31 C32 C33 14(2) . . . . ? C37 C32 C33 C34 1(2) . . . . ? C31 C32 C33 C34 -170.8(15) . . . . ? C32 C33 C34 C35 -2(2) . . . . ? C33 C34 C35 C36 -1(2) . . . . ? C33 C34 C35 C38 177.8(12) . . . . ? C34 C35 C36 C37 3(2) . . . . ? C38 C35 C36 C37 -175.3(14) . . . . ? C33 C32 C37 C36 1(3) . . . . ? C31 C32 C37 C36 173.4(15) . . . . ? C35 C36 C37 C32 -4(2) . . . . ? C34 C35 C38 C39 41.7(18) . . . . ? C36 C35 C38 C39 -140.0(13) . . . . ? C34 C35 C38 C43 -138.3(13) . . . . ? C36 C35 C38 C43 40.0(17) . . . . ? C43 C38 C39 C40 1(2) . . . . ? C35 C38 C39 C40 -179.4(12) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 C42 0(2) . . . . ? C40 C41 C42 C43 2(2) . . . . ? C41 C42 C43 C38 -3.2(19) . . . . ? C41 C42 C43 C44 174.1(12) . . . . ? C39 C38 C43 C42 1.7(17) . . . . ? C35 C38 C43 C42 -178.2(11) . . . . ? C39 C38 C43 C44 -175.3(11) . . . . ? C35 C38 C43 C44 4.7(17) . . . . ? C42 C43 C44 O14' 86(2) . . . . ? C38 C43 C44 O14' -96(2) . . . . ? C42 C43 C44 O13 -108.1(14) . . . . ? C38 C43 C44 O13 69.1(16) . . . . ? C42 C43 C44 O14 51(2) . . . . ? C38 C43 C44 O14 -131.9(18) . . . . ? O2 C7 O1 Pb2 -37(2) . . . . ? C1 C7 O1 Pb2 146.9(9) . . . . ? O15 Pb2 O1 C7 113.6(12) . . . . ? O13 Pb2 O1 C7 132.6(10) 1_545 . . . ? O11 Pb2 O1 C7 43.0(11) 2_457 . . . ? O9 Pb2 O1 C7 -169.4(11) . . . . ? O1 C7 O2 Pb1 -38.6(18) . . . . ? C1 C7 O2 Pb1 136.8(11) . . . . ? O2 Pb1 O2 C7 -128(100) 2_557 . . . ? O15 Pb1 O2 C7 33.8(9) . . . . ? O15 Pb1 O2 C7 -146.2(9) 2_557 . . . ? O11 Pb1 O2 C7 99.4(9) 2_457 . . . ? O11 Pb1 O2 C7 -80.6(9) 1_655 . . . ? O10 Pb1 O2 C7 146.3(9) 2_457 . . . ? O10 Pb1 O2 C7 -33.7(9) 1_655 . . . ? O4 C8 O3 Pb4 -0.9(16) . . . . ? C5 C8 O3 Pb4 -179.4(10) . . . . ? O6 Pb4 O3 C8 78.7(9) 2_556 . . . ? O2W Pb4 O3 C8 -161.4(11) 2_577 . . . ? O7 Pb4 O3 C8 132.2(10) 2_556 . . . ? O4 Pb4 O3 C8 0.5(8) . . . . ? O6 Pb4 O3 C8 17.2(11) 1_565 . . . ? O2W' Pb4 O3 C8 -147.3(11) 2_577 . . . ? C22 Pb4 O3 C8 105.1(10) 2_556 . . . ? O3 C8 O4 Pb4 0.8(14) . . . . ? C5 C8 O4 Pb4 179.3(12) . . . . ? O6 Pb4 O4 C8 -94.0(9) 2_556 . . . ? O3 Pb4 O4 C8 -0.5(8) . . . . ? O2W Pb4 O4 C8 29.3(15) 2_577 . . . ? O7 Pb4 O4 C8 -49.5(9) 2_556 . . . ? O6 Pb4 O4 C8 -165.0(9) 1_565 . . . ? O2W' Pb4 O4 C8 30.1(10) 2_577 . . . ? C22 Pb4 O4 C8 -72.7(9) 2_556 . . . ? C2 C3 O5 C9 -153.3(14) . . . . ? C4 C3 O5 C9 25(2) . . . . ? C10 C9 O5 C3 167.7(12) . . . . ? O7 C22 O6 Pb4 4.1(17) . . . 2_556 ? C21 C22 O6 Pb4 -171.0(14) . . . 2_556 ? O7 C22 O6 Pb4 149.0(13) . . . 1_545 ? C21 C22 O6 Pb4 -26(2) . . . 1_545 ? Pb4 C22 O6 Pb4 144.8(15) 2_556 . . 1_545 ? O6 C22 O7 Pb4 -3.9(16) . . . 2_556 ? C21 C22 O7 Pb4 171.2(15) . . . 2_556 ? O9 C29 O8 Pb3 -6.9(15) . . . . ? C23 C29 O8 Pb3 169.0(10) . . . . ? O15 Pb3 O8 C29 -57.0(9) . . . . ? O1W Pb3 O8 C29 -141.6(9) . . . . ? O9 Pb3 O8 C29 3.5(8) . . . . ? O10 Pb3 O8 C29 -122.3(9) 1_655 . . . ? O8 C29 O9 Pb2 100.7(15) . . . . ? C23 C29 O9 Pb2 -75.1(15) . . . . ? O8 C29 O9 Pb3 6.6(14) . . . . ? C23 C29 O9 Pb3 -169.3(10) . . . . ? O15 Pb2 O9 C29 -67.6(10) . . . . ? O13 Pb2 O9 C29 20.9(10) 1_545 . . . ? O11 Pb2 O9 C29 -54.7(12) 2_457 . . . ? O1 Pb2 O9 C29 -136.7(11) . . . . ? O15 Pb2 O9 Pb3 26.1(3) . . . . ? O13 Pb2 O9 Pb3 114.6(3) 1_545 . . . ? O11 Pb2 O9 Pb3 38.9(6) 2_457 . . . ? O1 Pb2 O9 Pb3 -43.0(3) . . . . ? O15 Pb3 O9 C29 110.1(8) . . . . ? O1W Pb3 O9 C29 34.8(9) . . . . ? O8 Pb3 O9 C29 -3.5(8) . . . . ? O10 Pb3 O9 C29 137.9(8) 1_655 . . . ? O15 Pb3 O9 Pb2 -26.9(2) . . . . ? O1W Pb3 O9 Pb2 -102.2(4) . . . . ? O8 Pb3 O9 Pb2 -140.5(5) . . . . ? O10 Pb3 O9 Pb2 0.9(6) 1_655 . . . ? O11 C30 O10 Pb3 -154(3) . . . 1_455 ? C25 C30 O10 Pb3 28(5) . . . 1_455 ? O11 C30 O10 Pb1 16.2(13) . . . 1_455 ? C25 C30 O10 Pb1 -161.4(11) . . . 1_455 ? O10 C30 O11 Pb2 -123.5(13) . . . 2_457 ? C25 C30 O11 Pb2 54.0(18) . . . 2_457 ? O10 C30 O11 Pb1 -16.4(14) . . . 1_455 ? C25 C30 O11 Pb1 161.1(10) . . . 1_455 ? C32 C31 O12 C27 162.4(13) . . . . ? C28 C27 O12 C31 -1(2) . . . . ? C26 C27 O12 C31 -179.2(15) . . . . ? O14' C44 O13 Pb2 -25(2) . . . 1_565 ? O14 C44 O13 Pb2 11(2) . . . 1_565 ? C43 C44 O13 Pb2 171.0(8) . . . 1_565 ? O13 C44 O14 O14' -111(3) . . . . ? C43 C44 O14 O14' 91(3) . . . . ? O13 C44 O14' O14 89(4) . . . . ? C43 C44 O14' O14 -107(3) . . . . ? O1W Pb3 O15 Pb2 151.5(3) . . . . ? O8 Pb3 O15 Pb2 76.3(3) . . . . ? O9 Pb3 O15 Pb2 31.5(3) . . . . ? O10 Pb3 O15 Pb2 -130.8(4) 1_655 . . . ? O1W Pb3 O15 Pb1 -100.4(3) . . . . ? O8 Pb3 O15 Pb1 -175.7(3) . . . . ? O9 Pb3 O15 Pb1 139.5(3) . . . . ? O10 Pb3 O15 Pb1 -22.8(3) 1_655 . . . ? O13 Pb2 O15 Pb3 -122.4(3) 1_545 . . . ? O11 Pb2 O15 Pb3 154.4(4) 2_457 . . . ? O9 Pb2 O15 Pb3 -32.8(3) . . . . ? O1 Pb2 O15 Pb3 49.2(4) . . . . ? O13 Pb2 O15 Pb1 121.1(3) 1_545 . . . ? O11 Pb2 O15 Pb1 37.8(3) 2_457 . . . ? O9 Pb2 O15 Pb1 -149.3(3) . . . . ? O1 Pb2 O15 Pb1 -67.4(3) . . . . ? O2 Pb1 O15 Pb3 110.0(3) 2_557 . . . ? O2 Pb1 O15 Pb3 -70.0(3) . . . . ? O15 Pb1 O15 Pb3 -160(100) 2_557 . . . ? O11 Pb1 O15 Pb3 -150.8(4) 2_457 . . . ? O11 Pb1 O15 Pb3 29.2(4) 1_655 . . . ? O10 Pb1 O15 Pb3 -156.7(3) 2_457 . . . ? O10 Pb1 O15 Pb3 23.3(3) 1_655 . . . ? O2 Pb1 O15 Pb2 -135.6(3) 2_557 . . . ? O2 Pb1 O15 Pb2 44.4(3) . . . . ? O15 Pb1 O15 Pb2 -45(100) 2_557 . . . ? O11 Pb1 O15 Pb2 -36.4(3) 2_457 . . . ? O11 Pb1 O15 Pb2 143.6(3) 1_655 . . . ? O10 Pb1 O15 Pb2 -42.3(4) 2_457 . . . ? O10 Pb1 O15 Pb2 137.7(4) 1_655 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1D O5W 0.87(2) 1.83(11) 2.51(2) 134(14) . O1W H1D O5W' 0.87(2) 1.94(6) 2.78(2) 164(17) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.025 _refine_diff_density_min -2.247 _refine_diff_density_rms 0.238 _database_code_depnum_ccdc_archive 'CCDC 938337' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H34 N6 O15 Zn4' _chemical_formula_sum 'C50 H34 N6 O15 Zn4' _chemical_formula_weight 1220.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.1130(11) _cell_length_b 24.003(3) _cell_length_c 10.3180(7) _cell_angle_alpha 90 _cell_angle_beta 97.813(8) _cell_angle_gamma 90 _cell_volume 2481.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2246 _cell_measurement_theta_min 3.1377 _cell_measurement_theta_max 29.2413 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1198 _exptl_absorpt_coefficient_mu 1.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5517 _exptl_absorpt_correction_T_max 0.5967 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10026 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4458 _reflns_number_gt 3095 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For O1 and Zn1, some anisotropic displacement ellipsoids were rather elongated which led us to use the DELU restraints. For C21, C21', C23, O8, O2W and O2W', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.0594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4458 _refine_ls_number_parameters 430 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.98240(9) 0.2500 0.55805(7) 0.0446(3) Uani 1 2 d SU . . Zn2 Zn 0.80529(6) 0.17428(3) 0.37795(5) 0.02940(19) Uani 1 1 d . . . Zn3 Zn 0.97713(8) 0.2500 0.23736(7) 0.0262(2) Uani 1 2 d S . . C1 C 0.7022(5) 0.1498(2) 0.7474(4) 0.0279(12) Uani 1 1 d . . . C2 C 0.7604(5) 0.1645(2) 0.8737(4) 0.0311(12) Uani 1 1 d . . . H2 H 0.8383 0.1855 0.8857 0.037 Uiso 1 1 calc R . . C3 C 0.7016(5) 0.1477(2) 0.9802(4) 0.0247(11) Uani 1 1 d . . . C4 C 0.5856(5) 0.1162(2) 0.9643(4) 0.0283(12) Uani 1 1 d . . . H4 H 0.5467 0.1051 1.0368 0.034 Uiso 1 1 calc R . . C5 C 0.5281(5) 0.1016(2) 0.8395(4) 0.0326(13) Uani 1 1 d . A . C6 C 0.5853(5) 0.1192(2) 0.7319(4) 0.0319(13) Uani 1 1 d . . . H6 H 0.5444 0.1104 0.6481 0.038 Uiso 1 1 calc R . . C7 C 0.7656(5) 0.1680(2) 0.6324(5) 0.0323(12) Uani 1 1 d . . . C8 C 0.7645(6) 0.1664(2) 1.1127(5) 0.0337(13) Uani 1 1 d . . . C9 C 0.3420(5) 0.0539(2) 0.9106(5) 0.0350(13) Uani 1 1 d . A . H9A H 0.3222 0.0861 0.9613 0.042 Uiso 1 1 calc R . . H9B H 0.3938 0.0278 0.9687 0.042 Uiso 1 1 calc R . . C10 C 0.2148(5) 0.0269(2) 0.8493(5) 0.0359(13) Uani 1 1 d . . . C11 C 0.1593(6) -0.0154(2) 0.9073(6) 0.0476(15) Uani 1 1 d . A . H11 H 0.2029 -0.0290 0.9861 0.057 Uiso 1 1 calc R . . C12 C 0.0410(6) -0.0393(2) 0.8553(6) 0.0483(16) Uani 1 1 d . . . H12 H 0.0067 -0.0684 0.9000 0.058 Uiso 1 1 calc R A . C13 C -0.0277(6) -0.0218(3) 0.7405(5) 0.0442(15) Uani 1 1 d . A . C14 C 0.0046(14) 0.0337(6) 0.6952(14) 0.041(4) Uani 0.492(9) 1 d P A 1 H14 H -0.0534 0.0523 0.6320 0.050 Uiso 0.492(9) 1 calc PR A 1 C15 C 0.1257(15) 0.0581(6) 0.7498(14) 0.040(4) Uani 0.492(9) 1 d P A 1 H15 H 0.1494 0.0934 0.7236 0.048 Uiso 0.492(9) 1 calc PR A 1 C20 C -0.399(3) -0.0461(10) 0.694(3) 0.079(9) Uani 0.492(9) 1 d P A 1 H20 H -0.4695 -0.0294 0.7285 0.094 Uiso 0.492(9) 1 calc PR A 1 C21 C -0.2623(14) -0.0243(6) 0.7321(13) 0.045(3) Uani 0.492(9) 1 d PU A 1 H21 H -0.2500 0.0062 0.7880 0.054 Uiso 0.492(9) 1 calc PR A 1 C22 C -0.0790(13) -0.1370(7) 0.6416(15) 0.031(3) Uani 0.492(9) 1 d P A 1 O7 O -0.1054(7) -0.1866(3) 0.6652(7) 0.041(3) Uani 0.492(9) 1 d P . 1 C14' C 0.0534(16) 0.0059(7) 0.6678(13) 0.052(4) Uani 0.508(9) 1 d P A 2 H14' H 0.0282 0.0079 0.5778 0.062 Uiso 0.508(9) 1 calc PR A 2 C15' C 0.1692(15) 0.0308(7) 0.7192(13) 0.047(4) Uani 0.508(9) 1 d P A 2 H15' H 0.2181 0.0508 0.6649 0.056 Uiso 0.508(9) 1 calc PR A 2 C20' C -0.398(3) -0.0250(9) 0.656(2) 0.054(6) Uani 0.508(9) 1 d P A 2 H20' H -0.4704 -0.0012 0.6581 0.064 Uiso 0.508(9) 1 calc PR A 2 C21' C -0.2786(13) -0.0061(6) 0.6860(12) 0.043(3) Uani 0.508(9) 1 d PU A 2 H21' H -0.2643 0.0315 0.7047 0.052 Uiso 0.508(9) 1 calc PR A 2 C22' C -0.0653(13) -0.1371(6) 0.5751(15) 0.027(3) Uani 0.508(9) 1 d P A 2 O7' O -0.1034(7) -0.1795(3) 0.5064(7) 0.043(3) Uani 0.508(9) 1 d P . 2 C16 C -0.1599(6) -0.0463(3) 0.6902(5) 0.0430(15) Uani 1 1 d . . . C17 C -0.1829(6) -0.0979(2) 0.6323(5) 0.0419(14) Uani 1 1 d . A . C18 C -0.3137(6) -0.1169(3) 0.5988(5) 0.0478(15) Uani 1 1 d . . . H18 H -0.3272 -0.1521 0.5619 0.057 Uiso 1 1 calc R A . C19 C -0.4227(7) -0.0858(3) 0.6178(6) 0.0586(18) Uani 1 1 d . A . C23 C 1.1571(13) 0.3164(5) 0.7498(12) 0.056(3) Uani 0.50 1 d PGU . . C24 C 1.2484(10) 0.2399(16) 0.7215(8) 0.036(9) Uani 0.50 1 d PG . . C25 C 1.4505(7) 0.2500 0.8882(6) 0.0298(17) Uani 1 2 d S . . C26 C 1.4482(7) 0.2500 1.0378(7) 0.042(2) Uani 1 2 d S . . C27 C 1.1533(5) 0.3184(2) 1.0851(4) 0.045(3) Uani 0.50 1 d PGU . . C28 C 1.2453(6) 0.2400(2) 1.1485(4) 0.035(3) Uani 0.50 1 d PG . . N1 N 1.1405(6) 0.2684(3) 0.6797(5) 0.031(2) Uani 0.50 1 d PG . . N2 N 1.2670(5) 0.31570(17) 0.8304(4) 0.051(3) Uani 0.50 1 d PGU . . N3 N 1.3280(5) 0.2665(2) 0.8140(4) 0.029(2) Uani 0.50 1 d PG . . N4 N 1.1391(6) 0.2725(2) 1.1550(4) 0.032(2) Uani 0.50 1 d PG . . N5 N 1.2682(5) 0.31430(16) 1.0353(4) 0.055(3) Uani 0.50 1 d PG . . N6 N 1.3250(4) 0.2658(2) 1.0745(4) 0.035(3) Uani 0.50 1 d PG . . O1 O 0.8777(4) 0.18986(17) 0.6518(3) 0.0479(9) Uani 1 1 d U . . O2 O 0.7017(4) 0.15825(17) 0.5198(3) 0.0417(10) Uani 1 1 d . . . O3 O 0.8769(4) 0.18850(17) 1.1220(3) 0.0464(10) Uani 1 1 d . . . O4 O 0.6989(4) 0.15843(16) 1.2080(3) 0.0395(9) Uani 1 1 d . . . O5 O 0.4156(4) 0.07037(18) 0.8093(3) 0.0536(12) Uani 1 1 d . . . O6 O 0.0426(4) -0.12137(15) 0.6098(3) 0.0390(9) Uani 1 1 d . . . O8 O 0.8762(4) 0.2500 0.3867(4) 0.0225(10) Uani 1 2 d SU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0202(5) 0.0938(8) 0.0191(4) 0.000 -0.0001(3) 0.000 Zn2 0.0310(4) 0.0405(4) 0.0165(3) -0.0006(3) 0.0025(2) -0.0072(3) Zn3 0.0210(5) 0.0378(5) 0.0201(4) 0.000 0.0039(3) 0.000 C1 0.029(3) 0.032(3) 0.023(2) 0.004(2) 0.005(2) 0.001(2) C2 0.024(3) 0.034(3) 0.034(3) -0.002(2) -0.002(2) -0.006(2) C3 0.023(3) 0.030(3) 0.021(2) -0.002(2) 0.002(2) -0.006(2) C4 0.034(3) 0.031(3) 0.021(2) 0.003(2) 0.007(2) -0.002(2) C5 0.030(3) 0.041(3) 0.026(2) -0.005(2) 0.003(2) -0.015(3) C6 0.030(3) 0.041(3) 0.023(2) 0.000(2) -0.002(2) -0.013(2) C7 0.023(3) 0.042(3) 0.032(3) 0.006(2) 0.003(2) -0.003(2) C8 0.034(4) 0.031(3) 0.033(3) -0.004(2) -0.007(2) 0.003(3) C9 0.035(3) 0.037(3) 0.034(3) -0.001(3) 0.007(2) -0.009(3) C10 0.038(3) 0.040(3) 0.030(3) -0.008(3) 0.008(2) -0.016(3) C11 0.037(4) 0.047(4) 0.056(3) 0.017(3) -0.006(3) -0.009(3) C12 0.033(4) 0.041(4) 0.069(4) 0.018(3) -0.002(3) -0.015(3) C13 0.040(4) 0.050(4) 0.041(3) -0.011(3) 0.002(3) -0.018(3) C14 0.028(8) 0.039(9) 0.053(8) 0.013(7) -0.012(6) 0.005(6) C15 0.047(9) 0.020(8) 0.053(8) 0.003(7) 0.007(7) -0.008(6) C20 0.048(12) 0.07(2) 0.13(2) -0.013(16) 0.067(14) -0.009(14) C21 0.045(4) 0.045(4) 0.045(4) -0.0003(10) 0.0062(11) -0.0001(10) C22 0.033(8) 0.037(9) 0.023(7) 0.000(8) 0.002(6) 0.008(6) O7 0.037(5) 0.031(5) 0.056(5) 0.010(4) 0.003(4) -0.002(4) C14' 0.053(11) 0.063(11) 0.039(7) 0.001(8) 0.004(7) -0.023(8) C15' 0.056(10) 0.046(10) 0.041(7) -0.008(7) 0.015(7) -0.031(8) C20' 0.037(9) 0.031(11) 0.094(15) -0.010(9) 0.011(10) -0.018(8) C21' 0.043(3) 0.043(3) 0.043(3) -0.0001(10) 0.0057(11) 0.0000(10) C22' 0.033(8) 0.025(7) 0.027(7) 0.000(7) 0.015(6) 0.001(5) O7' 0.034(5) 0.037(5) 0.056(5) -0.024(4) 0.000(4) -0.004(3) C16 0.035(4) 0.054(4) 0.041(3) -0.011(3) 0.007(3) -0.014(3) C17 0.031(4) 0.043(4) 0.048(3) 0.011(3) -0.008(3) -0.001(3) C18 0.038(4) 0.044(4) 0.057(3) -0.004(3) -0.009(3) -0.006(3) C19 0.039(4) 0.075(5) 0.062(4) -0.024(4) 0.009(3) -0.010(4) C23 0.056(4) 0.056(4) 0.056(3) -0.0006(10) 0.0067(11) -0.0004(10) C24 0.026(5) 0.05(3) 0.032(4) 0.001(6) 0.004(4) -0.001(7) C25 0.019(4) 0.042(5) 0.026(3) 0.000 -0.003(3) 0.000 C26 0.021(4) 0.071(6) 0.036(4) 0.000 0.014(3) 0.000 C27 0.045(3) 0.045(3) 0.045(3) 0.0008(10) 0.0071(11) -0.0002(10) C28 0.019(5) 0.042(10) 0.042(5) 0.006(6) 0.002(4) -0.009(6) N1 0.021(5) 0.028(6) 0.041(4) -0.005(3) -0.005(4) -0.001(3) N2 0.051(3) 0.051(3) 0.052(3) -0.0011(10) 0.0056(11) 0.0004(10) N3 0.029(5) 0.021(7) 0.039(4) -0.008(3) 0.007(4) 0.008(3) N4 0.031(5) 0.030(5) 0.033(4) 0.003(3) 0.003(4) 0.006(4) N5 0.058(7) 0.031(6) 0.080(7) 0.020(5) 0.027(6) 0.014(5) N6 0.027(5) 0.044(10) 0.036(4) 0.004(4) 0.008(4) 0.002(4) O1 0.028(2) 0.071(3) 0.043(2) 0.0030(18) -0.0031(17) -0.0038(18) O2 0.030(2) 0.073(3) 0.0219(17) 0.0088(18) 0.0036(15) -0.0123(19) O3 0.035(2) 0.064(3) 0.039(2) -0.0227(19) -0.0024(18) -0.012(2) O4 0.040(2) 0.058(3) 0.0191(16) -0.0037(17) -0.0020(16) -0.0065(19) O5 0.056(3) 0.077(3) 0.0307(18) -0.018(2) 0.0164(19) -0.046(2) O6 0.032(3) 0.040(2) 0.044(2) -0.0055(18) 0.0022(19) -0.0066(18) O8 0.0226(13) 0.0238(13) 0.0211(12) 0.000 0.0034(9) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O8 1.940(4) . ? Zn1 N1 1.945(6) . ? Zn1 N1 1.945(6) 4_565 ? Zn1 O1 2.102(4) 4_565 ? Zn1 O1 2.102(4) . ? Zn1 O7' 2.243(7) 3_656 ? Zn1 O7' 2.243(7) 2_656 ? Zn1 Zn2 3.0099(9) . ? Zn1 Zn2 3.0099(9) 4_565 ? Zn2 O2 1.950(3) . ? Zn2 O8 1.9513(17) . ? Zn2 O4 1.966(3) 1_554 ? Zn2 O6 1.985(4) 3_656 ? Zn2 Zn3 3.0189(8) . ? Zn3 O8 1.961(4) . ? Zn3 N4 2.018(14) 4_564 ? Zn3 N4 2.018(14) 1_554 ? Zn3 O3 2.072(4) 1_554 ? Zn3 O3 2.072(4) 4_564 ? Zn3 O7 2.158(7) 2_656 ? Zn3 O7 2.158(7) 3_656 ? Zn3 Zn2 3.0189(8) 4_565 ? C1 C6 1.382(7) . ? C1 C2 1.401(6) . ? C1 C7 1.489(6) . ? C2 C3 1.378(6) . ? C2 H2 0.9300 . ? C3 C4 1.387(7) . ? C3 C8 1.497(6) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 O5 1.362(6) . ? C5 C6 1.386(6) . ? C6 H6 0.9300 . ? C7 O1 1.240(6) . ? C7 O2 1.272(6) . ? C8 O3 1.246(6) . ? C8 O4 1.273(6) . ? C9 O5 1.418(6) . ? C9 C10 1.501(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.340(7) . ? C10 C15' 1.362(14) . ? C10 C15 1.474(15) . ? C11 C12 1.369(8) . ? C11 H11 0.9300 . ? C12 C13 1.356(8) . ? C12 H12 0.9300 . ? C13 C14' 1.357(15) . ? C13 C14 1.463(15) . ? C13 C16 1.488(8) . ? C14 C15 1.404(19) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C20 C19 1.24(3) . ? C20 C21 1.48(3) . ? C20 H20 0.9300 . ? C21 C16 1.289(14) . ? C21 H21 0.9300 . ? C22 O7 1.250(17) . ? C22 O6 1.367(15) . ? C22 C17 1.403(15) . ? O7 Zn3 2.158(7) 3_656 ? C14' C15' 1.357(18) . ? C14' H14' 0.9300 . ? C15' H15' 0.9300 . ? C20' C21' 1.29(3) . ? C20' C19 1.52(2) . ? C20' H20' 0.9300 . ? C21' C16 1.535(15) . ? C21' H21' 0.9300 . ? C22' O6 1.164(13) . ? C22' O7' 1.269(15) . ? C22' C17 1.685(15) . ? O7' Zn1 2.243(7) 3_656 ? C16 C17 1.382(8) . ? C17 C18 1.397(8) . ? C18 C19 1.367(9) . ? C18 H18 0.9300 . ? C23 N2 1.294(13) . ? C23 N1 1.359(14) . ? C23 C24 1.68(3) 4_565 ? C24 C24 0.48(7) 4_565 ? C24 N1 1.135(13) 4_565 ? C24 N3 1.172(11) 4_565 ? C24 N1 1.31(2) . ? C24 N3 1.32(2) . ? C24 C23 1.68(3) 4_565 ? C24 N2 1.74(3) 4_565 ? C25 N3 1.421(8) 4_565 ? C25 N3 1.421(8) . ? C25 C26 1.547(9) . ? C26 N6 1.403(8) 4_565 ? C26 N6 1.403(8) . ? C27 N4 1.3363(19) . ? C27 N5 1.3364(19) . ? C27 C28 1.758(8) 4_565 ? C28 C28 0.482(10) 4_565 ? C28 N4 1.125(3) 4_565 ? C28 N6 1.1914(17) 4_565 ? C28 N6 1.3362(19) . ? C28 N4 1.3363(19) . ? C28 C27 1.758(8) 4_565 ? C28 N5 1.785(6) 4_565 ? N1 N1 0.882(12) 4_565 ? N1 C24 1.14(5) 4_565 ? N2 N3 1.354(2) . ? N2 C24 1.74(5) 4_565 ? N3 N3 0.790(10) 4_565 ? N3 C24 1.17(7) 4_565 ? N4 N4 1.078(12) 4_565 ? N4 C28 1.125(3) 4_565 ? N4 Zn3 2.018(5) 1_556 ? N5 N6 1.3362(19) . ? N5 C28 1.785(7) 4_565 ? N6 N6 0.759(10) 4_565 ? N6 C28 1.1914(18) 4_565 ? O3 Zn3 2.072(4) 1_556 ? O4 Zn2 1.966(3) 1_556 ? O6 Zn2 1.985(4) 3_656 ? O8 Zn2 1.9513(17) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Zn1 N1 153.3(2) . . ? O8 Zn1 N1 153.3(2) . 4_565 ? N1 Zn1 N1 26.2(4) . 4_565 ? O8 Zn1 O1 99.67(13) . 4_565 ? N1 Zn1 O1 88.2(2) . 4_565 ? N1 Zn1 O1 106.3(2) 4_565 4_565 ? O8 Zn1 O1 99.67(13) . . ? N1 Zn1 O1 106.3(2) . . ? N1 Zn1 O1 88.2(2) 4_565 . ? O1 Zn1 O1 86.7(2) 4_565 . ? O8 Zn1 O7' 89.3(2) . 3_656 ? N1 Zn1 O7' 85.9(3) . 3_656 ? N1 Zn1 O7' 65.5(2) 4_565 3_656 ? O1 Zn1 O7' 169.8(2) 4_565 3_656 ? O1 Zn1 O7' 87.0(2) . 3_656 ? O8 Zn1 O7' 89.3(2) . 2_656 ? N1 Zn1 O7' 65.5(2) . 2_656 ? N1 Zn1 O7' 85.9(3) 4_565 2_656 ? O1 Zn1 O7' 87.0(2) 4_565 2_656 ? O1 Zn1 O7' 169.8(2) . 2_656 ? O7' Zn1 O7' 98.1(4) 3_656 2_656 ? O8 Zn1 Zn2 39.47(4) . . ? N1 Zn1 Zn2 154.63(18) . . ? N1 Zn1 Zn2 129.03(19) 4_565 . ? O1 Zn1 Zn2 113.82(11) 4_565 . ? O1 Zn1 Zn2 64.83(10) . . ? O7' Zn1 Zn2 70.37(18) 3_656 . ? O7' Zn1 Zn2 125.17(19) 2_656 . ? O8 Zn1 Zn2 39.47(4) . 4_565 ? N1 Zn1 Zn2 129.03(18) . 4_565 ? N1 Zn1 Zn2 154.6(2) 4_565 4_565 ? O1 Zn1 Zn2 64.83(10) 4_565 4_565 ? O1 Zn1 Zn2 113.82(11) . 4_565 ? O7' Zn1 Zn2 125.17(19) 3_656 4_565 ? O7' Zn1 Zn2 70.37(18) 2_656 4_565 ? Zn2 Zn1 Zn2 74.29(3) . 4_565 ? O2 Zn2 O8 112.36(16) . . ? O2 Zn2 O4 110.28(15) . 1_554 ? O8 Zn2 O4 112.00(16) . 1_554 ? O2 Zn2 O6 108.45(16) . 3_656 ? O8 Zn2 O6 108.44(16) . 3_656 ? O4 Zn2 O6 104.97(15) 1_554 3_656 ? O2 Zn2 Zn1 89.49(11) . . ? O8 Zn2 Zn1 39.19(11) . . ? O4 Zn2 Zn1 151.07(11) 1_554 . ? O6 Zn2 Zn1 87.48(11) 3_656 . ? O2 Zn2 Zn3 151.92(12) . . ? O8 Zn2 Zn3 39.61(11) . . ? O4 Zn2 Zn3 88.22(11) 1_554 . ? O6 Zn2 Zn3 85.65(11) 3_656 . ? Zn1 Zn2 Zn3 66.42(2) . . ? O8 Zn3 N4 150.4(4) . 4_564 ? O8 Zn3 N4 150.4(4) . 1_554 ? N4 Zn3 N4 31.0(8) 4_564 1_554 ? O8 Zn3 O3 100.66(14) . 1_554 ? N4 Zn3 O3 86.0(4) 4_564 1_554 ? N4 Zn3 O3 108.1(4) 1_554 1_554 ? O8 Zn3 O3 100.66(14) . 4_564 ? N4 Zn3 O3 108.1(4) 4_564 4_564 ? N4 Zn3 O3 86.0(4) 1_554 4_564 ? O3 Zn3 O3 90.9(2) 1_554 4_564 ? O8 Zn3 O7 88.8(2) . 2_656 ? N4 Zn3 O7 85.0(5) 4_564 2_656 ? N4 Zn3 O7 62.4(4) 1_554 2_656 ? O3 Zn3 O7 170.5(2) 1_554 2_656 ? O3 Zn3 O7 88.9(2) 4_564 2_656 ? O8 Zn3 O7 88.8(2) . 3_656 ? N4 Zn3 O7 62.4(4) 4_564 3_656 ? N4 Zn3 O7 85.0(4) 1_554 3_656 ? O3 Zn3 O7 88.9(2) 1_554 3_656 ? O3 Zn3 O7 170.5(2) 4_564 3_656 ? O7 Zn3 O7 89.7(4) 2_656 3_656 ? O8 Zn3 Zn2 39.38(4) . . ? N4 Zn3 Zn2 126.5(4) 4_564 . ? N4 Zn3 Zn2 156.4(4) 1_554 . ? O3 Zn3 Zn2 65.07(10) 1_554 . ? O3 Zn3 Zn2 115.87(12) 4_564 . ? O7 Zn3 Zn2 123.4(2) 2_656 . ? O7 Zn3 Zn2 72.6(2) 3_656 . ? O8 Zn3 Zn2 39.38(4) . 4_565 ? N4 Zn3 Zn2 156.4(4) 4_564 4_565 ? N4 Zn3 Zn2 126.5(4) 1_554 4_565 ? O3 Zn3 Zn2 115.87(11) 1_554 4_565 ? O3 Zn3 Zn2 65.07(10) 4_564 4_565 ? O7 Zn3 Zn2 72.6(2) 2_656 4_565 ? O7 Zn3 Zn2 123.4(2) 3_656 4_565 ? Zn2 Zn3 Zn2 74.04(3) . 4_565 ? C6 C1 C2 119.1(4) . . ? C6 C1 C7 121.2(4) . . ? C2 C1 C7 119.7(5) . . ? C3 C2 C1 119.8(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.0(4) . . ? C2 C3 C8 117.7(4) . . ? C4 C3 C8 121.3(4) . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? O5 C5 C4 125.7(4) . . ? O5 C5 C6 114.3(4) . . ? C4 C5 C6 119.9(5) . . ? C1 C6 C5 120.9(4) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? O1 C7 O2 124.4(4) . . ? O1 C7 C1 118.6(4) . . ? O2 C7 C1 116.9(4) . . ? O3 C8 O4 124.8(4) . . ? O3 C8 C3 117.9(5) . . ? O4 C8 C3 117.3(5) . . ? O5 C9 C10 108.4(4) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C11 C10 C15' 112.7(7) . . ? C11 C10 C15 116.3(7) . . ? C15' C10 C15 35.5(6) . . ? C11 C10 C9 121.7(5) . . ? C15' C10 C9 122.8(7) . . ? C15 C10 C9 118.8(7) . . ? C10 C11 C12 122.6(5) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 121.9(5) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14' 111.0(8) . . ? C12 C13 C14 116.8(7) . . ? C14' C13 C14 36.9(7) . . ? C12 C13 C16 120.7(5) . . ? C14' C13 C16 125.6(7) . . ? C14 C13 C16 118.6(7) . . ? C15 C14 C13 118.1(10) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C14 C15 C10 119.0(11) . . ? C14 C15 H15 120.5 . . ? C10 C15 H15 120.5 . . ? C19 C20 C21 122(2) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 122.0(15) . . ? C16 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? O7 C22 O6 122.1(11) . . ? O7 C22 C17 118.1(12) . . ? O6 C22 C17 119.3(12) . . ? C22 O7 Zn3 129.1(8) . 3_656 ? C15' C14' C13 123.6(12) . . ? C15' C14' H14' 118.2 . . ? C13 C14' H14' 118.2 . . ? C14' C15' C10 120.9(12) . . ? C14' C15' H15' 119.5 . . ? C10 C15' H15' 119.5 . . ? C21' C20' C19 121(2) . . ? C21' C20' H20' 119.6 . . ? C19 C20' H20' 119.6 . . ? C20' C21' C16 119.4(14) . . ? C20' C21' H21' 120.3 . . ? C16 C21' H21' 120.3 . . ? O6 C22' O7' 129.3(12) . . ? O6 C22' C17 112.8(11) . . ? O7' C22' C17 117.8(10) . . ? C22' O7' Zn1 129.3(8) . 3_656 ? C21 C16 C17 114.6(8) . . ? C21 C16 C13 116.5(7) . . ? C17 C16 C13 126.6(6) . . ? C21 C16 C21' 24.7(7) . . ? C17 C16 C21' 117.7(7) . . ? C13 C16 C21' 115.0(7) . . ? C16 C17 C18 119.8(5) . . ? C16 C17 C22 119.3(8) . . ? C18 C17 C22 118.4(8) . . ? C16 C17 C22' 124.5(7) . . ? C18 C17 C22' 114.9(7) . . ? C22 C17 C22' 24.8(5) . . ? C19 C18 C17 122.8(6) . . ? C19 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? C20 C19 C18 114.9(14) . . ? C20 C19 C20' 24.1(17) . . ? C18 C19 C20' 117.0(11) . . ? N2 C23 N1 111.4(10) . . ? N2 C23 C24 70(2) . 4_565 ? N1 C23 C24 42(2) . 4_565 ? C24 C24 N1 100(6) 4_565 4_565 ? C24 C24 N3 98(8) 4_565 4_565 ? N1 C24 N3 144(2) 4_565 4_565 ? C24 C24 N1 59(5) 4_565 . ? N1 C24 N1 41.5(8) 4_565 . ? N3 C24 N1 142(2) 4_565 . ? C24 C24 N3 61(8) 4_565 . ? N1 C24 N3 144.8(19) 4_565 . ? N3 C24 N3 36.2(6) 4_565 . ? N1 C24 N3 113(3) . . ? C24 C24 C23 143.4(10) 4_565 4_565 ? N1 C24 C23 53.4(13) 4_565 4_565 ? N3 C24 C23 94.9(19) 4_565 4_565 ? N1 C24 C23 91.4(11) . 4_565 ? N3 C24 C23 123.7(12) . 4_565 ? C24 C24 N2 140(8) 4_565 4_565 ? N1 C24 N2 97(2) 4_565 4_565 ? N3 C24 N2 51.0(11) 4_565 4_565 ? N1 C24 N2 128.7(12) . 4_565 ? N3 C24 N2 84.4(8) . 4_565 ? C23 C24 N2 44.4(10) 4_565 4_565 ? N3 C25 N3 32.3(4) 4_565 . ? N3 C25 C26 114.1(5) 4_565 . ? N3 C25 C26 114.1(5) . . ? N6 C26 N6 31.4(5) 4_565 . ? N6 C26 C25 113.8(6) 4_565 . ? N6 C26 C25 113.8(6) . . ? N4 C27 N5 108.0 . . ? N4 C27 C28 39.78(11) . 4_565 ? N5 C27 C28 68.91(7) . 4_565 ? C28 C28 N4 105.4(6) 4_565 4_565 ? C28 C28 N6 96.7(5) 4_565 4_565 ? N4 C28 N6 137.9(5) 4_565 4_565 ? C28 C28 N6 62.3 4_565 . ? N4 C28 N6 144.3(3) 4_565 . ? N6 C28 N6 34.3(5) 4_565 . ? C28 C28 N4 54.3 4_565 . ? N4 C28 N4 51.1(6) 4_565 . ? N6 C28 N4 135.9(4) 4_565 . ? N6 C28 N4 108.0 . . ? C28 C28 C27 142.8(4) 4_565 4_565 ? N4 C28 C27 49.5(3) 4_565 4_565 ? N6 C28 C27 92.2(5) 4_565 4_565 ? N6 C28 C27 119.18(19) . 4_565 ? N4 C28 C27 95.5(4) . 4_565 ? C28 C28 N5 136.9(2) 4_565 4_565 ? N4 C28 N5 93.2(6) 4_565 4_565 ? N6 C28 N5 48.5(3) 4_565 4_565 ? N6 C28 N5 79.8(2) . 4_565 ? N4 C28 N5 129.46(5) . 4_565 ? C27 C28 N5 44.3(4) 4_565 4_565 ? N1 N1 C24 79.9(16) 4_565 4_565 ? N1 N1 C24 58.6(15) 4_565 . ? C24 N1 C24 21(3) 4_565 . ? N1 N1 C23 148.0(6) 4_565 . ? C24 N1 C23 84(2) 4_565 . ? C24 N1 C23 103.3(14) . . ? N1 N1 Zn1 76.9(3) 4_565 . ? C24 N1 Zn1 150(2) 4_565 . ? C24 N1 Zn1 132.0(14) . . ? C23 N1 Zn1 124.6(7) . . ? C23 N2 N3 107.3(6) . . ? C23 N2 C24 65.6(17) . 4_565 ? N3 N2 C24 42.3(17) . 4_565 ? N3 N3 C24 82.5(15) 4_565 4_565 ? N3 N3 C24 61.3(15) 4_565 . ? C24 N3 C24 21(3) 4_565 . ? N3 N3 N2 150.8 4_565 . ? C24 N3 N2 86.7(13) 4_565 . ? C24 N3 N2 105.5(13) . . ? N3 N3 C25 73.9(3) 4_565 . ? C24 N3 C25 148.7(12) 4_565 . ? C24 N3 C25 130.9(14) . . ? N2 N3 C25 123.6(3) . . ? N4 N4 C28 74.6(5) 4_565 4_565 ? N4 N4 C28 54.3 4_565 . ? C28 N4 C28 20.4(5) 4_565 . ? N4 N4 C27 145.6 4_565 . ? C28 N4 C27 90.8(4) 4_565 . ? C28 N4 C27 108.0 . . ? N4 N4 Zn3 74.5(3) 4_565 1_556 ? C28 N4 Zn3 142.2(6) 4_565 1_556 ? C28 N4 Zn3 124.7(3) . 1_556 ? C27 N4 Zn3 126.9(3) . 1_556 ? N6 N5 C27 108.0 . . ? N6 N5 C28 41.87(15) . 4_565 ? C27 N5 C28 66.78(12) . 4_565 ? N6 N6 C28 83.3(5) 4_565 4_565 ? N6 N6 N5 150.6 4_565 . ? C28 N6 N5 89.7(4) 4_565 . ? N6 N6 C28 62.3 4_565 . ? C28 N6 C28 21.0(5) 4_565 . ? N5 N6 C28 108.0 . . ? N6 N6 C26 74.3(3) 4_565 . ? C28 N6 C26 147.7(5) 4_565 . ? N5 N6 C26 121.0(3) . . ? C28 N6 C26 131.0(3) . . ? C7 O1 Zn1 136.3(3) . . ? C7 O2 Zn2 113.0(3) . . ? C8 O3 Zn3 135.8(3) . 1_556 ? C8 O4 Zn2 112.3(3) . 1_556 ? C5 O5 C9 119.4(4) . . ? C22' O6 C22 31.7(5) . . ? C22' O6 Zn2 119.9(7) . 3_656 ? C22 O6 Zn2 121.5(7) . 3_656 ? Zn1 O8 Zn2 101.34(12) . . ? Zn1 O8 Zn2 101.34(12) . 4_565 ? Zn2 O8 Zn2 137.3(2) . 4_565 ? Zn1 O8 Zn3 115.7(2) . . ? Zn2 O8 Zn3 101.00(12) . . ? Zn2 O8 Zn3 101.00(12) 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Zn1 Zn2 O2 -127.8(2) . . . . ? N1 Zn1 Zn2 O2 96.3(4) . . . . ? N1 Zn1 Zn2 O2 86.7(3) 4_565 . . . ? O1 Zn1 Zn2 O2 -52.12(16) 4_565 . . . ? O1 Zn1 Zn2 O2 21.84(17) . . . . ? O7' Zn1 Zn2 O2 117.9(2) 3_656 . . . ? O7' Zn1 Zn2 O2 -156.0(3) 2_656 . . . ? Zn2 Zn1 Zn2 O2 -104.73(12) 4_565 . . . ? N1 Zn1 Zn2 O8 -135.9(4) . . . . ? N1 Zn1 Zn2 O8 -145.5(3) 4_565 . . . ? O1 Zn1 Zn2 O8 75.7(2) 4_565 . . . ? O1 Zn1 Zn2 O8 149.6(2) . . . . ? O7' Zn1 Zn2 O8 -114.3(3) 3_656 . . . ? O7' Zn1 Zn2 O8 -28.2(3) 2_656 . . . ? Zn2 Zn1 Zn2 O8 23.07(19) 4_565 . . . ? O8 Zn1 Zn2 O4 6.6(3) . . . 1_554 ? N1 Zn1 Zn2 O4 -129.3(5) . . . 1_554 ? N1 Zn1 Zn2 O4 -138.9(3) 4_565 . . 1_554 ? O1 Zn1 Zn2 O4 82.3(3) 4_565 . . 1_554 ? O1 Zn1 Zn2 O4 156.3(3) . . . 1_554 ? O7' Zn1 Zn2 O4 -107.6(3) 3_656 . . 1_554 ? O7' Zn1 Zn2 O4 -21.6(3) 2_656 . . 1_554 ? Zn2 Zn1 Zn2 O4 29.7(2) 4_565 . . 1_554 ? O8 Zn1 Zn2 O6 123.7(2) . . . 3_656 ? N1 Zn1 Zn2 O6 -12.2(4) . . . 3_656 ? N1 Zn1 Zn2 O6 -21.8(3) 4_565 . . 3_656 ? O1 Zn1 Zn2 O6 -160.61(15) 4_565 . . 3_656 ? O1 Zn1 Zn2 O6 -86.65(16) . . . 3_656 ? O7' Zn1 Zn2 O6 9.4(2) 3_656 . . 3_656 ? O7' Zn1 Zn2 O6 95.5(2) 2_656 . . 3_656 ? Zn2 Zn1 Zn2 O6 146.78(10) 4_565 . . 3_656 ? O8 Zn1 Zn2 Zn3 37.36(19) . . . . ? N1 Zn1 Zn2 Zn3 -98.6(4) . . . . ? N1 Zn1 Zn2 Zn3 -108.2(2) 4_565 . . . ? O1 Zn1 Zn2 Zn3 113.04(12) 4_565 . . . ? O1 Zn1 Zn2 Zn3 -173.00(12) . . . . ? O7' Zn1 Zn2 Zn3 -76.9(2) 3_656 . . . ? O7' Zn1 Zn2 Zn3 9.1(2) 2_656 . . . ? Zn2 Zn1 Zn2 Zn3 60.43(2) 4_565 . . . ? O2 Zn2 Zn3 O8 -4.0(3) . . . . ? O4 Zn2 Zn3 O8 128.7(2) 1_554 . . . ? O6 Zn2 Zn3 O8 -126.1(2) 3_656 . . . ? Zn1 Zn2 Zn3 O8 -36.98(19) . . . . ? O2 Zn2 Zn3 N4 139.5(5) . . . 4_564 ? O8 Zn2 Zn3 N4 143.5(5) . . . 4_564 ? O4 Zn2 Zn3 N4 -87.8(5) 1_554 . . 4_564 ? O6 Zn2 Zn3 N4 17.4(5) 3_656 . . 4_564 ? Zn1 Zn2 Zn3 N4 106.6(5) . . . 4_564 ? O2 Zn2 Zn3 N4 125.5(9) . . . 1_554 ? O8 Zn2 Zn3 N4 129.5(9) . . . 1_554 ? O4 Zn2 Zn3 N4 -101.8(9) 1_554 . . 1_554 ? O6 Zn2 Zn3 N4 3.4(9) 3_656 . . 1_554 ? Zn1 Zn2 Zn3 N4 92.5(9) . . . 1_554 ? O2 Zn2 Zn3 O3 -156.6(3) . . . 1_554 ? O8 Zn2 Zn3 O3 -152.6(2) . . . 1_554 ? O4 Zn2 Zn3 O3 -23.88(17) 1_554 . . 1_554 ? O6 Zn2 Zn3 O3 81.29(16) 3_656 . . 1_554 ? Zn1 Zn2 Zn3 O3 170.44(13) . . . 1_554 ? O2 Zn2 Zn3 O3 -78.5(3) . . . 4_564 ? O8 Zn2 Zn3 O3 -74.5(2) . . . 4_564 ? O4 Zn2 Zn3 O3 54.18(17) 1_554 . . 4_564 ? O6 Zn2 Zn3 O3 159.34(16) 3_656 . . 4_564 ? Zn1 Zn2 Zn3 O3 -111.51(12) . . . 4_564 ? O2 Zn2 Zn3 O7 28.5(3) . . . 2_656 ? O8 Zn2 Zn3 O7 32.6(3) . . . 2_656 ? O4 Zn2 Zn3 O7 161.3(3) 1_554 . . 2_656 ? O6 Zn2 Zn3 O7 -93.6(3) 3_656 . . 2_656 ? Zn1 Zn2 Zn3 O7 -4.4(2) . . . 2_656 ? O2 Zn2 Zn3 O7 106.3(3) . . . 3_656 ? O8 Zn2 Zn3 O7 110.3(3) . . . 3_656 ? O4 Zn2 Zn3 O7 -121.0(2) 1_554 . . 3_656 ? O6 Zn2 Zn3 O7 -15.8(2) 3_656 . . 3_656 ? Zn1 Zn2 Zn3 O7 73.3(2) . . . 3_656 ? O2 Zn2 Zn3 Zn2 -27.3(2) . . . 4_565 ? O8 Zn2 Zn3 Zn2 -23.28(19) . . . 4_565 ? O4 Zn2 Zn3 Zn2 105.43(11) 1_554 . . 4_565 ? O6 Zn2 Zn3 Zn2 -149.41(10) 3_656 . . 4_565 ? Zn1 Zn2 Zn3 Zn2 -60.26(2) . . . 4_565 ? C6 C1 C2 C3 1.0(8) . . . . ? C7 C1 C2 C3 179.8(5) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? C1 C2 C3 C8 -177.7(5) . . . . ? C2 C3 C4 C5 -0.1(8) . . . . ? C8 C3 C4 C5 177.7(5) . . . . ? C3 C4 C5 O5 179.2(5) . . . . ? C3 C4 C5 C6 -1.2(8) . . . . ? C2 C1 C6 C5 -2.3(8) . . . . ? C7 C1 C6 C5 178.9(5) . . . . ? O5 C5 C6 C1 -178.0(5) . . . . ? C4 C5 C6 C1 2.4(8) . . . . ? C6 C1 C7 O1 -172.1(5) . . . . ? C2 C1 C7 O1 9.1(8) . . . . ? C6 C1 C7 O2 5.6(8) . . . . ? C2 C1 C7 O2 -173.2(5) . . . . ? C2 C3 C8 O3 -10.9(7) . . . . ? C4 C3 C8 O3 171.3(5) . . . . ? C2 C3 C8 O4 169.1(5) . . . . ? C4 C3 C8 O4 -8.7(7) . . . . ? O5 C9 C10 C11 145.8(6) . . . . ? O5 C9 C10 C15' -13.8(12) . . . . ? O5 C9 C10 C15 -55.2(9) . . . . ? C15' C10 C11 C12 -20.8(12) . . . . ? C15 C10 C11 C12 18.2(11) . . . . ? C9 C10 C11 C12 177.7(6) . . . . ? C10 C11 C12 C13 0.4(10) . . . . ? C11 C12 C13 C14' 21.1(12) . . . . ? C11 C12 C13 C14 -18.9(12) . . . . ? C11 C12 C13 C16 -176.4(6) . . . . ? C12 C13 C14 C15 17.8(17) . . . . ? C14' C13 C14 C15 -71.9(16) . . . . ? C16 C13 C14 C15 175.8(11) . . . . ? C13 C14 C15 C10 0(2) . . . . ? C11 C10 C15 C14 -17.9(16) . . . . ? C15' C10 C15 C14 74.8(17) . . . . ? C9 C10 C15 C14 -178.0(11) . . . . ? C19 C20 C21 C16 -2(3) . . . . ? O6 C22 O7 Zn3 35.9(19) . . . 3_656 ? C17 C22 O7 Zn3 -152.0(7) . . . 3_656 ? C12 C13 C14' C15' -23(2) . . . . ? C14 C13 C14' C15' 84(2) . . . . ? C16 C13 C14' C15' 175.5(13) . . . . ? C13 C14' C15' C10 3(3) . . . . ? C11 C10 C15' C14' 18.9(19) . . . . ? C15 C10 C15' C14' -85(2) . . . . ? C9 C10 C15' C14' -179.8(13) . . . . ? C19 C20' C21' C16 -3(3) . . . . ? O6 C22' O7' Zn1 9(2) . . . 3_656 ? C17 C22' O7' Zn1 -168.0(6) . . . 3_656 ? C20 C21 C16 C17 -13.5(19) . . . . ? C20 C21 C16 C13 -177.5(14) . . . . ? C20 C21 C16 C21' 90(2) . . . . ? C12 C13 C16 C21 86.0(11) . . . . ? C14' C13 C16 C21 -114.2(13) . . . . ? C14 C13 C16 C21 -71.1(12) . . . . ? C12 C13 C16 C17 -75.8(8) . . . . ? C14' C13 C16 C17 84.0(13) . . . . ? C14 C13 C16 C17 127.1(9) . . . . ? C12 C13 C16 C21' 113.4(8) . . . . ? C14' C13 C16 C21' -86.8(12) . . . . ? C14 C13 C16 C21' -43.7(11) . . . . ? C20' C21' C16 C21 -74(2) . . . . ? C20' C21' C16 C17 15.1(18) . . . . ? C20' C21' C16 C13 -173.2(14) . . . . ? C21 C16 C17 C18 13.2(10) . . . . ? C13 C16 C17 C18 175.3(5) . . . . ? C21' C16 C17 C18 -14.2(9) . . . . ? C21 C16 C17 C22 -148.6(12) . . . . ? C13 C16 C17 C22 13.5(11) . . . . ? C21' C16 C17 C22 -175.9(11) . . . . ? C21 C16 C17 C22' -177.3(11) . . . . ? C13 C16 C17 C22' -15.2(10) . . . . ? C21' C16 C17 C22' 155.4(10) . . . . ? O7 C22 C17 C16 137.4(10) . . . . ? O6 C22 C17 C16 -50.2(15) . . . . ? O7 C22 C17 C18 -24.6(16) . . . . ? O6 C22 C17 C18 147.8(9) . . . . ? O7 C22 C17 C22' -113(3) . . . . ? O6 C22 C17 C22' 59(2) . . . . ? O6 C22' C17 C16 13.2(15) . . . . ? O7' C22' C17 C16 -169.3(9) . . . . ? O6 C22' C17 C18 -176.9(9) . . . . ? O7' C22' C17 C18 0.7(14) . . . . ? O6 C22' C17 C22 -73(2) . . . . ? O7' C22' C17 C22 105(3) . . . . ? C16 C17 C18 C19 1.6(9) . . . . ? C22 C17 C18 C19 163.5(9) . . . . ? C22' C17 C18 C19 -168.9(7) . . . . ? C21 C20 C19 C18 16(3) . . . . ? C21 C20 C19 C20' -84(5) . . . . ? C17 C18 C19 C20 -16.5(16) . . . . ? C17 C18 C19 C20' 10.2(13) . . . . ? C21' C20' C19 C20 82(5) . . . . ? C21' C20' C19 C18 -9(2) . . . . ? N3 C25 C26 N6 -0.5(3) 4_565 . . 4_565 ? N3 C25 C26 N6 34.9(4) . . . 4_565 ? N3 C25 C26 N6 -34.9(4) 4_565 . . . ? N3 C25 C26 N6 0.5(3) . . . . ? C24 C24 N1 N1 180(8) 4_565 . . 4_565 ? N3 C24 N1 N1 -122(4) 4_565 . . 4_565 ? N3 C24 N1 N1 -149.8(14) . . . 4_565 ? C23 C24 N1 N1 -22.2(6) 4_565 . . 4_565 ? N2 C24 N1 N1 -48.4(19) 4_565 . . 4_565 ? N1 C24 N1 C24 180(8) 4_565 . . 4_565 ? N3 C24 N1 C24 58(9) 4_565 . . 4_565 ? N3 C24 N1 C24 30(8) . . . 4_565 ? C23 C24 N1 C24 158(8) 4_565 . . 4_565 ? N2 C24 N1 C24 132(8) 4_565 . . 4_565 ? C24 C24 N1 C23 -29(8) 4_565 . . . ? N1 C24 N1 C23 151.3(6) 4_565 . . . ? N3 C24 N1 C23 29(4) 4_565 . . . ? N3 C24 N1 C23 1.5(16) . . . . ? C23 C24 N1 C23 129.1(11) 4_565 . . . ? N2 C24 N1 C23 103(2) 4_565 . . . ? C24 C24 N1 Zn1 155(8) 4_565 . . . ? N1 C24 N1 Zn1 -24.7(10) 4_565 . . . ? N3 C24 N1 Zn1 -147(3) 4_565 . . . ? N3 C24 N1 Zn1 -174.5(6) . . . . ? C23 C24 N1 Zn1 -46.8(9) 4_565 . . . ? N2 C24 N1 Zn1 -73.1(16) 4_565 . . . ? N2 C23 N1 N1 49.3(17) . . . 4_565 ? C24 C23 N1 N1 61(3) 4_565 . . 4_565 ? N2 C23 N1 C24 -12(3) . . . 4_565 ? N2 C23 N1 C24 -1.4(13) . . . . ? C24 C23 N1 C24 10(3) 4_565 . . . ? N2 C23 N1 Zn1 175.0(5) . . . . ? C24 C23 N1 Zn1 -174(3) 4_565 . . . ? O8 Zn1 N1 N1 -117.6(4) . . . 4_565 ? O1 Zn1 N1 N1 134.28(18) 4_565 . . 4_565 ? O1 Zn1 N1 N1 48.20(18) . . . 4_565 ? O7' Zn1 N1 N1 -37.4(2) 3_656 . . 4_565 ? O7' Zn1 N1 N1 -138.2(3) 2_656 . . 4_565 ? Zn2 Zn1 N1 N1 -17.1(3) . . . 4_565 ? Zn2 Zn1 N1 N1 -170.7(2) 4_565 . . 4_565 ? O8 Zn1 N1 C24 -78(5) . . . 4_565 ? N1 Zn1 N1 C24 39(5) 4_565 . . 4_565 ? O1 Zn1 N1 C24 174(5) 4_565 . . 4_565 ? O1 Zn1 N1 C24 88(5) . . . 4_565 ? O7' Zn1 N1 C24 2(5) 3_656 . . 4_565 ? O7' Zn1 N1 C24 -99(5) 2_656 . . 4_565 ? Zn2 Zn1 N1 C24 22(5) . . . 4_565 ? Zn2 Zn1 N1 C24 -131(5) 4_565 . . 4_565 ? O8 Zn1 N1 C24 -96.1(11) . . . . ? N1 Zn1 N1 C24 21.5(11) 4_565 . . . ? O1 Zn1 N1 C24 155.7(11) 4_565 . . . ? O1 Zn1 N1 C24 69.7(11) . . . . ? O7' Zn1 N1 C24 -16.0(11) 3_656 . . . ? O7' Zn1 N1 C24 -116.8(11) 2_656 . . . ? Zn2 Zn1 N1 C24 4.4(13) . . . . ? Zn2 Zn1 N1 C24 -149.2(10) 4_565 . . . ? O8 Zn1 N1 C23 88.7(9) . . . . ? N1 Zn1 N1 C23 -153.8(7) 4_565 . . . ? O1 Zn1 N1 C23 -19.5(8) 4_565 . . . ? O1 Zn1 N1 C23 -105.6(8) . . . . ? O7' Zn1 N1 C23 168.8(8) 3_656 . . . ? O7' Zn1 N1 C23 68.0(8) 2_656 . . . ? Zn2 Zn1 N1 C23 -170.8(6) . . . . ? Zn2 Zn1 N1 C23 35.5(8) 4_565 . . . ? N1 C23 N2 N3 0.8(10) . . . . ? C24 C23 N2 N3 -7.3(14) 4_565 . . . ? N1 C23 N2 C24 8.2(16) . . . 4_565 ? C24 C24 N3 N3 180(3) 4_565 . . 4_565 ? N1 C24 N3 N3 115(5) 4_565 . . 4_565 ? N1 C24 N3 N3 150.7(14) . . . 4_565 ? C23 C24 N3 N3 42.7(17) 4_565 . . 4_565 ? N2 C24 N3 N3 20.9(4) 4_565 . . 4_565 ? N1 C24 N3 C24 -65(5) 4_565 . . 4_565 ? N3 C24 N3 C24 180(3) 4_565 . . 4_565 ? N1 C24 N3 C24 -29(3) . . . 4_565 ? C23 C24 N3 C24 -137(3) 4_565 . . 4_565 ? N2 C24 N3 C24 -159(3) 4_565 . . 4_565 ? C24 C24 N3 N2 28(3) 4_565 . . . ? N1 C24 N3 N2 -36(5) 4_565 . . . ? N3 C24 N3 N2 -151.7(2) 4_565 . . . ? N1 C24 N3 N2 -1.0(15) . . . . ? C23 C24 N3 N2 -109.0(19) 4_565 . . . ? N2 C24 N3 N2 -130.8(6) 4_565 . . . ? C24 C24 N3 C25 -153(3) 4_565 . . . ? N1 C24 N3 C25 142(4) 4_565 . . . ? N3 C24 N3 C25 26.6(11) 4_565 . . . ? N1 C24 N3 C25 177.3(7) . . . . ? C23 C24 N3 C25 69.4(15) 4_565 . . . ? N2 C24 N3 C25 47.6(9) 4_565 . . . ? C23 N2 N3 N3 -58.2(6) . . . 4_565 ? C24 N2 N3 N3 -68.1(15) 4_565 . . 4_565 ? C23 N2 N3 C24 10.0(16) . . . 4_565 ? C23 N2 N3 C24 0.1(10) . . . . ? C24 N2 N3 C24 -9.9(19) 4_565 . . . ? C23 N2 N3 C25 -178.4(8) . . . . ? C24 N2 N3 C25 171.6(16) 4_565 . . . ? C26 C25 N3 N3 -97.4(3) . . . 4_565 ? N3 C25 N3 C24 -42(3) 4_565 . . 4_565 ? C26 C25 N3 C24 -140(3) . . . 4_565 ? N3 C25 N3 C24 -24.2(12) 4_565 . . . ? C26 C25 N3 C24 -121.6(11) . . . . ? N3 C25 N3 N2 153.95(15) 4_565 . . . ? C26 C25 N3 N2 56.5(4) . . . . ? C28 C28 N4 N4 180.0 4_565 . . 4_565 ? N6 C28 N4 N4 122.5(5) 4_565 . . 4_565 ? N6 C28 N4 N4 146.6 . . . 4_565 ? C27 C28 N4 N4 23.53(14) 4_565 . . 4_565 ? N5 C28 N4 N4 55.1(3) 4_565 . . 4_565 ? N4 C28 N4 C28 180.0 4_565 . . 4_565 ? N6 C28 N4 C28 -57.5(5) 4_565 . . 4_565 ? N6 C28 N4 C28 -33.4 . . . 4_565 ? C27 C28 N4 C28 -156.47(13) 4_565 . . 4_565 ? N5 C28 N4 C28 -124.9(3) 4_565 . . 4_565 ? C28 C28 N4 C27 33.3 4_565 . . . ? N4 C28 N4 C27 -146.7 4_565 . . . ? N6 C28 N4 C27 -24.1(5) 4_565 . . . ? N6 C28 N4 C27 0.0 . . . . ? C27 C28 N4 C27 -123.13(14) 4_565 . . . ? N5 C28 N4 C27 -91.5(3) 4_565 . . . ? C28 C28 N4 Zn3 -153.8(3) 4_565 . . 1_556 ? N4 C28 N4 Zn3 26.2(3) 4_565 . . 1_556 ? N6 C28 N4 Zn3 148.7(6) 4_565 . . 1_556 ? N6 C28 N4 Zn3 172.8(3) . . . 1_556 ? C27 C28 N4 Zn3 49.7(3) 4_565 . . 1_556 ? N5 C28 N4 Zn3 81.3(4) 4_565 . . 1_556 ? N5 C27 N4 N4 -52.2 . . . 4_565 ? C28 C27 N4 N4 -63.2(3) 4_565 . . 4_565 ? N5 C27 N4 C28 11.0(3) . . . 4_565 ? N5 C27 N4 C28 0.0 . . . . ? C28 C27 N4 C28 -11.0(3) 4_565 . . . ? N5 C27 N4 Zn3 -172.6(3) . . . 1_556 ? C28 C27 N4 Zn3 176.4(4) 4_565 . . 1_556 ? N4 C27 N5 N6 0.0 . . . . ? C28 C27 N5 N6 7.54(19) 4_565 . . . ? N4 C27 N5 C28 -7.54(19) . . . 4_565 ? C27 N5 N6 N6 65.3 . . . 4_565 ? C28 N5 N6 N6 75.7(2) 4_565 . . 4_565 ? C27 N5 N6 C28 -10.4(2) . . . 4_565 ? C27 N5 N6 C28 0.0 . . . . ? C28 N5 N6 C28 10.4(2) 4_565 . . . ? C27 N5 N6 C26 -179.6(4) . . . . ? C28 N5 N6 C26 -169.2(5) 4_565 . . . ? C28 C28 N6 N6 180.0 4_565 . . 4_565 ? N4 C28 N6 N6 -102.6(10) 4_565 . . 4_565 ? N4 C28 N6 N6 -149.7 . . . 4_565 ? C27 C28 N6 N6 -42.5(5) 4_565 . . 4_565 ? N5 C28 N6 N6 -21.37(11) 4_565 . . 4_565 ? N4 C28 N6 C28 77.4(10) 4_565 . . 4_565 ? N6 C28 N6 C28 180.0 4_565 . . 4_565 ? N4 C28 N6 C28 30.3 . . . 4_565 ? C27 C28 N6 C28 137.5(5) 4_565 . . 4_565 ? N5 C28 N6 C28 158.63(11) 4_565 . . 4_565 ? C28 C28 N6 N5 -30.3 4_565 . . . ? N4 C28 N6 N5 47.2(10) 4_565 . . . ? N6 C28 N6 N5 149.7 4_565 . . . ? N4 C28 N6 N5 0.0 . . . . ? C27 C28 N6 N5 107.3(5) 4_565 . . . ? N5 C28 N6 N5 128.37(11) 4_565 . . . ? C28 C28 N6 C26 149.3(5) 4_565 . . . ? N4 C28 N6 C26 -133.2(10) 4_565 . . . ? N6 C28 N6 C26 -30.7(5) 4_565 . . . ? N4 C28 N6 C26 179.6(5) . . . . ? C27 C28 N6 C26 -73.1(5) 4_565 . . . ? N5 C28 N6 C26 -52.0(5) 4_565 . . . ? C25 C26 N6 N6 97.1(3) . . . 4_565 ? N6 C26 N6 C28 48.0(10) 4_565 . . 4_565 ? C25 C26 N6 C28 145.1(8) . . . 4_565 ? N6 C26 N6 N5 -152.47(14) 4_565 . . . ? C25 C26 N6 N5 -55.3(4) . . . . ? N6 C26 N6 C28 28.0(4) 4_565 . . . ? C25 C26 N6 C28 125.1(3) . . . . ? O2 C7 O1 Zn1 33.3(9) . . . . ? C1 C7 O1 Zn1 -149.2(4) . . . . ? O8 Zn1 O1 C7 -17.7(6) . . . . ? N1 Zn1 O1 C7 168.8(5) . . . . ? N1 Zn1 O1 C7 -172.0(6) 4_565 . . . ? O1 Zn1 O1 C7 81.6(5) 4_565 . . . ? O7' Zn1 O1 C7 -106.4(6) 3_656 . . . ? O7' Zn1 O1 C7 133.4(12) 2_656 . . . ? Zn2 Zn1 O1 C7 -36.7(5) . . . . ? Zn2 Zn1 O1 C7 21.0(6) 4_565 . . . ? O1 C7 O2 Zn2 5.8(7) . . . . ? C1 C7 O2 Zn2 -171.8(4) . . . . ? O8 Zn2 O2 C7 -54.0(4) . . . . ? O4 Zn2 O2 C7 -179.7(4) 1_554 . . . ? O6 Zn2 O2 C7 65.9(4) 3_656 . . . ? Zn1 Zn2 O2 C7 -21.3(4) . . . . ? Zn3 Zn2 O2 C7 -51.2(5) . . . . ? O4 C8 O3 Zn3 -33.1(9) . . . 1_556 ? C3 C8 O3 Zn3 147.0(4) . . . 1_556 ? O3 C8 O4 Zn2 -8.8(7) . . . 1_556 ? C3 C8 O4 Zn2 171.1(3) . . . 1_556 ? C4 C5 O5 C9 4.9(9) . . . . ? C6 C5 O5 C9 -174.7(5) . . . . ? C10 C9 O5 C5 172.6(5) . . . . ? O7' C22' O6 C22 -126(3) . . . . ? C17 C22' O6 C22 51.5(18) . . . . ? O7' C22' O6 Zn2 -23.1(19) . . . 3_656 ? C17 C22' O6 Zn2 154.1(5) . . . 3_656 ? O7 C22 O6 C22' 88(2) . . . . ? C17 C22 O6 C22' -84(2) . . . . ? O7 C22 O6 Zn2 -8.4(16) . . . 3_656 ? C17 C22 O6 Zn2 179.5(7) . . . 3_656 ? N1 Zn1 O8 Zn2 138.5(4) . . . . ? N1 Zn1 O8 Zn2 77.9(5) 4_565 . . . ? O1 Zn1 O8 Zn2 -115.95(17) 4_565 . . . ? O1 Zn1 O8 Zn2 -27.6(2) . . . . ? O7' Zn1 O8 Zn2 59.2(2) 3_656 . . . ? O7' Zn1 O8 Zn2 157.2(2) 2_656 . . . ? Zn2 Zn1 O8 Zn2 -143.6(3) 4_565 . . . ? N1 Zn1 O8 Zn2 -77.9(5) . . . 4_565 ? N1 Zn1 O8 Zn2 -138.5(5) 4_565 . . 4_565 ? O1 Zn1 O8 Zn2 27.6(2) 4_565 . . 4_565 ? O1 Zn1 O8 Zn2 115.95(17) . . . 4_565 ? O7' Zn1 O8 Zn2 -157.2(2) 3_656 . . 4_565 ? O7' Zn1 O8 Zn2 -59.2(2) 2_656 . . 4_565 ? Zn2 Zn1 O8 Zn2 143.6(3) . . . 4_565 ? N1 Zn1 O8 Zn3 30.3(4) . . . . ? N1 Zn1 O8 Zn3 -30.3(5) 4_565 . . . ? O1 Zn1 O8 Zn3 135.85(12) 4_565 . . . ? O1 Zn1 O8 Zn3 -135.85(12) . . . . ? O7' Zn1 O8 Zn3 -49.04(19) 3_656 . . . ? O7' Zn1 O8 Zn3 49.04(19) 2_656 . . . ? Zn2 Zn1 O8 Zn3 -108.20(14) . . . . ? Zn2 Zn1 O8 Zn3 108.20(14) 4_565 . . . ? O2 Zn2 O8 Zn1 58.7(2) . . . . ? O4 Zn2 O8 Zn1 -176.54(15) 1_554 . . . ? O6 Zn2 O8 Zn1 -61.2(2) 3_656 . . . ? Zn3 Zn2 O8 Zn1 -119.3(3) . . . . ? O2 Zn2 O8 Zn2 -62.2(3) . . . 4_565 ? O4 Zn2 O8 Zn2 62.6(3) 1_554 . . 4_565 ? O6 Zn2 O8 Zn2 178.0(3) 3_656 . . 4_565 ? Zn1 Zn2 O8 Zn2 -120.9(4) . . . 4_565 ? Zn3 Zn2 O8 Zn2 119.8(4) . . . 4_565 ? O2 Zn2 O8 Zn3 177.96(15) . . . . ? O4 Zn2 O8 Zn3 -57.3(2) 1_554 . . . ? O6 Zn2 O8 Zn3 58.1(2) 3_656 . . . ? Zn1 Zn2 O8 Zn3 119.3(3) . . . . ? N4 Zn3 O8 Zn1 32.8(9) 4_564 . . . ? N4 Zn3 O8 Zn1 -32.8(8) 1_554 . . . ? O3 Zn3 O8 Zn1 133.54(12) 1_554 . . . ? O3 Zn3 O8 Zn1 -133.54(12) 4_564 . . . ? O7 Zn3 O8 Zn1 -44.9(2) 2_656 . . . ? O7 Zn3 O8 Zn1 44.9(2) 3_656 . . . ? Zn2 Zn3 O8 Zn1 108.40(14) . . . . ? Zn2 Zn3 O8 Zn1 -108.40(14) 4_565 . . . ? N4 Zn3 O8 Zn2 -75.6(9) 4_564 . . . ? N4 Zn3 O8 Zn2 -141.2(8) 1_554 . . . ? O3 Zn3 O8 Zn2 25.1(2) 1_554 . . . ? O3 Zn3 O8 Zn2 118.06(17) 4_564 . . . ? O7 Zn3 O8 Zn2 -153.3(3) 2_656 . . . ? O7 Zn3 O8 Zn2 -63.5(2) 3_656 . . . ? Zn2 Zn3 O8 Zn2 143.2(3) 4_565 . . . ? N4 Zn3 O8 Zn2 141.2(8) 4_564 . . 4_565 ? N4 Zn3 O8 Zn2 75.6(9) 1_554 . . 4_565 ? O3 Zn3 O8 Zn2 -118.06(17) 1_554 . . 4_565 ? O3 Zn3 O8 Zn2 -25.1(2) 4_564 . . 4_565 ? O7 Zn3 O8 Zn2 63.5(2) 2_656 . . 4_565 ? O7 Zn3 O8 Zn2 153.3(3) 3_656 . . 4_565 ? Zn2 Zn3 O8 Zn2 -143.2(3) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.580 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 938338' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H46 N4 O16 Zn2' _chemical_formula_sum 'C58 H46 N4 O16 Zn2' _chemical_formula_weight 1185.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5387(8) _cell_length_b 10.7309(8) _cell_length_c 12.8111(14) _cell_angle_alpha 105.788(8) _cell_angle_beta 108.142(8) _cell_angle_gamma 98.441(6) _cell_volume 1281.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1671 _cell_measurement_theta_min 3.1196 _cell_measurement_theta_max 29.0732 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7641 _exptl_absorpt_correction_T_max 0.8305 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7807 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4512 _reflns_number_gt 3149 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For O1W, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.4243P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4512 _refine_ls_number_parameters 361 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.55462(5) 0.38270(5) 0.50733(5) 0.02845(19) Uani 1 1 d . . . C1 C 0.1659(5) 0.1103(5) 0.0038(5) 0.0378(13) Uani 1 1 d . . . C2 C 0.2467(5) 0.1789(5) 0.1204(5) 0.0386(13) Uani 1 1 d . . . H2 H 0.3284 0.1574 0.1545 0.046 Uiso 1 1 calc R . . C3 C 0.2061(4) 0.2796(5) 0.1862(4) 0.0317(12) Uani 1 1 d . . . C4 C 0.0844(4) 0.3102(5) 0.1349(4) 0.0338(12) Uani 1 1 d . . . H4 H 0.0584 0.3798 0.1778 0.041 Uiso 1 1 calc R . . C5 C 0.0004(5) 0.2380(5) 0.0198(4) 0.0368(13) Uani 1 1 d . . . C6 C 0.0417(5) 0.1385(5) -0.0461(4) 0.0355(12) Uani 1 1 d . . . H6 H -0.0139 0.0907 -0.1236 0.043 Uiso 1 1 calc R . . C7 C 0.2195(8) 0.0101(6) -0.0644(6) 0.0575(17) Uani 1 1 d . . . C8 C 0.3018(4) 0.3580(5) 0.3080(4) 0.0333(12) Uani 1 1 d . . . C9 C -0.1735(5) 0.3559(6) 0.0293(5) 0.0501(15) Uani 1 1 d . . . H9A H -0.1111 0.4437 0.0559 0.060 Uiso 1 1 calc R . . H9B H -0.1780 0.3347 0.0972 0.060 Uiso 1 1 calc R . . C10 C -0.3152(5) 0.3558(6) -0.0470(4) 0.0390(13) Uani 1 1 d . . . C11 C -0.4250(5) 0.2450(6) -0.0884(5) 0.0488(15) Uani 1 1 d . . . H11 H -0.4107 0.1676 -0.0724 0.059 Uiso 1 1 calc R . . C12 C -0.5565(5) 0.2480(5) -0.1538(5) 0.0420(13) Uani 1 1 d . . . H12 H -0.6293 0.1726 -0.1803 0.050 Uiso 1 1 calc R . . C13 C -0.5813(4) 0.3615(5) -0.1803(4) 0.0319(11) Uani 1 1 d . . . C14 C -0.4704(5) 0.4722(5) -0.1385(4) 0.0359(12) Uani 1 1 d . . . H14 H -0.4842 0.5498 -0.1543 0.043 Uiso 1 1 calc R . . C15 C -0.3394(5) 0.4689(5) -0.0734(4) 0.0385(13) Uani 1 1 d . . . H15 H -0.2664 0.5441 -0.0469 0.046 Uiso 1 1 calc R . . C16 C -0.7241(4) 0.3664(4) -0.2452(4) 0.0302(11) Uani 1 1 d . . . C17 C -0.8321(5) 0.3111(5) -0.2162(5) 0.0387(13) Uani 1 1 d . . . H17 H -0.8133 0.2677 -0.1615 0.046 Uiso 1 1 calc R . . C18 C -0.9652(5) 0.3195(6) -0.2669(5) 0.0477(15) Uani 1 1 d . . . H18 H -1.0353 0.2802 -0.2475 0.057 Uiso 1 1 calc R . . C19 C -0.9943(5) 0.3851(6) -0.3452(5) 0.0508(16) Uani 1 1 d . . . H19 H -1.0838 0.3922 -0.3783 0.061 Uiso 1 1 calc R . . C20 C -0.8901(5) 0.4411(5) -0.3751(5) 0.0453(14) Uani 1 1 d . . . H20 H -0.9098 0.4874 -0.4274 0.054 Uiso 1 1 calc R . . C21 C -0.7557(4) 0.4292(4) -0.3283(4) 0.0303(11) Uani 1 1 d . . . C22 C -0.6565(4) 0.4753(5) -0.3813(4) 0.0291(11) Uani 1 1 d . . . C23 C 0.6570(4) 0.2054(5) 0.6465(5) 0.0344(12) Uani 1 1 d . . . H23 H 0.6616 0.2669 0.7154 0.041 Uiso 1 1 calc R . . C24 C 0.6970(4) 0.0971(4) 0.6423(4) 0.0202(10) Uani 1 1 d . . . H24 H 0.7351 0.0669 0.7037 0.024 Uiso 1 1 calc R . . C25 C 0.6185(4) 0.1125(5) 0.4685(5) 0.0322(12) Uani 1 1 d . . . H25 H 0.5933 0.0918 0.3883 0.039 Uiso 1 1 calc R . . C26 C 0.7188(5) -0.0822(5) 0.4876(5) 0.0381(13) Uani 1 1 d . . . H26A H 0.6584 -0.1348 0.4080 0.046 Uiso 1 1 calc R . . H26B H 0.7156 -0.1370 0.5361 0.046 Uiso 1 1 calc R . . C27 C 0.8653(4) -0.0412(4) 0.4929(5) 0.0329(12) Uani 1 1 d . . . C28 C 0.8944(5) 0.0254(6) 0.4230(5) 0.0510(16) Uani 1 1 d . . . H28 H 0.8224 0.0430 0.3699 0.061 Uiso 1 1 calc R . . C29 C 1.0285(5) 0.0676(5) 0.4289(5) 0.0460(14) Uani 1 1 d . . . H29 H 1.0460 0.1131 0.3805 0.055 Uiso 1 1 calc R . . N1 N 0.6075(3) 0.2216(3) 0.5409(3) 0.0277(9) Uani 1 1 d . . . N2 N 0.6709(3) 0.0382(4) 0.5287(4) 0.0287(9) Uani 1 1 d . . . O1 O 0.3874(3) 0.3017(3) 0.3586(3) 0.0462(10) Uani 1 1 d . . . O2 O 0.2944(3) 0.4745(3) 0.3519(3) 0.0422(9) Uani 1 1 d . . . O3 O 0.3408(5) 0.0032(5) -0.0232(4) 0.0752(14) Uani 1 1 d . . . O4 O 0.1371(5) -0.0653(4) -0.1673(4) 0.0748(14) Uani 1 1 d . . . H4O H 0.1767 -0.1164 -0.1970 0.112 Uiso 1 1 calc R . . O5 O -0.1245(3) 0.2582(4) -0.0371(3) 0.0488(10) Uani 1 1 d . . . O6 O -0.5790(3) 0.4031(3) -0.4034(3) 0.0364(8) Uani 1 1 d . . . O7 O -0.6617(3) 0.5821(3) -0.4038(3) 0.0400(9) Uani 1 1 d . . . O1W O 0.6604(6) 0.1807(6) 0.2332(5) 0.1140(19) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0260(3) 0.0294(3) 0.0313(4) 0.0128(2) 0.0081(2) 0.0117(2) C1 0.044(3) 0.035(3) 0.040(3) 0.015(3) 0.021(3) 0.012(2) C2 0.034(3) 0.042(3) 0.042(3) 0.021(3) 0.010(2) 0.012(2) C3 0.026(2) 0.033(3) 0.034(3) 0.013(2) 0.007(2) 0.005(2) C4 0.031(2) 0.040(3) 0.028(3) 0.009(2) 0.008(2) 0.012(2) C5 0.029(3) 0.047(3) 0.033(3) 0.015(3) 0.008(2) 0.010(2) C6 0.039(3) 0.034(3) 0.031(3) 0.010(2) 0.011(2) 0.007(2) C7 0.089(5) 0.050(4) 0.061(5) 0.030(3) 0.050(4) 0.028(4) C8 0.024(2) 0.040(3) 0.035(3) 0.016(3) 0.007(2) 0.004(2) C9 0.039(3) 0.069(4) 0.036(3) 0.010(3) 0.006(3) 0.025(3) C10 0.031(3) 0.062(3) 0.022(3) 0.013(3) 0.007(2) 0.016(3) C11 0.047(3) 0.051(3) 0.049(4) 0.023(3) 0.010(3) 0.020(3) C12 0.034(3) 0.046(3) 0.047(4) 0.026(3) 0.011(3) 0.005(2) C13 0.031(2) 0.042(3) 0.029(3) 0.017(2) 0.013(2) 0.013(2) C14 0.034(3) 0.039(3) 0.038(3) 0.018(2) 0.012(2) 0.011(2) C15 0.030(3) 0.049(3) 0.031(3) 0.011(3) 0.007(2) 0.008(2) C16 0.028(2) 0.027(2) 0.036(3) 0.009(2) 0.013(2) 0.008(2) C17 0.032(3) 0.051(3) 0.038(3) 0.022(3) 0.014(2) 0.006(2) C18 0.034(3) 0.063(4) 0.051(4) 0.020(3) 0.022(3) 0.011(3) C19 0.025(3) 0.073(4) 0.054(4) 0.022(3) 0.013(3) 0.013(3) C20 0.032(3) 0.061(3) 0.050(4) 0.029(3) 0.012(3) 0.022(3) C21 0.028(2) 0.030(2) 0.034(3) 0.012(2) 0.012(2) 0.008(2) C22 0.025(2) 0.036(3) 0.023(3) 0.011(2) 0.004(2) 0.008(2) C23 0.031(2) 0.036(3) 0.034(3) 0.011(2) 0.008(2) 0.009(2) C24 0.024(2) 0.025(2) 0.015(2) 0.0134(19) 0.0037(18) 0.0119(19) C25 0.026(2) 0.042(3) 0.033(3) 0.015(2) 0.012(2) 0.015(2) C26 0.034(3) 0.031(3) 0.052(4) 0.011(2) 0.019(2) 0.013(2) C27 0.028(2) 0.024(2) 0.045(3) 0.005(2) 0.016(2) 0.009(2) C28 0.031(3) 0.066(4) 0.068(4) 0.036(3) 0.017(3) 0.022(3) C29 0.041(3) 0.061(4) 0.057(4) 0.037(3) 0.025(3) 0.023(3) N1 0.0242(19) 0.028(2) 0.036(3) 0.0112(19) 0.0133(18) 0.0136(17) N2 0.0262(19) 0.029(2) 0.041(3) 0.018(2) 0.0172(18) 0.0153(17) O1 0.0390(19) 0.047(2) 0.038(2) 0.0134(18) -0.0040(17) 0.0133(17) O2 0.0291(18) 0.041(2) 0.041(2) 0.0030(17) 0.0013(16) 0.0080(16) O3 0.078(3) 0.088(3) 0.085(4) 0.033(3) 0.044(3) 0.054(3) O4 0.103(3) 0.072(3) 0.053(3) 0.008(3) 0.036(3) 0.039(3) O5 0.0304(18) 0.074(3) 0.031(2) 0.0069(19) 0.0019(16) 0.0228(19) O6 0.0347(18) 0.0404(19) 0.044(2) 0.0177(17) 0.0204(16) 0.0177(16) O7 0.050(2) 0.0409(19) 0.047(2) 0.0263(18) 0.0276(18) 0.0226(17) O1W 0.117(2) 0.114(2) 0.114(2) 0.0363(11) 0.0449(12) 0.0331(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.006(4) . ? Zn1 O1 2.012(3) . ? Zn1 O2 2.031(3) 2_666 ? Zn1 O7 2.063(3) 2_565 ? Zn1 O6 2.073(3) 1_656 ? Zn1 Zn1 2.9448(11) 2_666 ? C1 C6 1.383(7) . ? C1 C2 1.387(7) . ? C1 C7 1.487(8) . ? C2 C3 1.389(7) . ? C2 H2 0.9300 . ? C3 C4 1.379(6) . ? C3 C8 1.488(7) . ? C4 C5 1.387(7) . ? C4 H4 0.9300 . ? C5 O5 1.372(5) . ? C5 C6 1.384(7) . ? C6 H6 0.9300 . ? C7 O3 1.244(7) . ? C7 O4 1.284(7) . ? C8 O2 1.249(6) . ? C8 O1 1.268(5) . ? C9 O5 1.427(6) . ? C9 C10 1.509(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.380(7) . ? C10 C15 1.383(7) . ? C11 C12 1.389(7) . ? C11 H11 0.9300 . ? C12 C13 1.390(7) . ? C12 H12 0.9300 . ? C13 C14 1.386(6) . ? C13 C16 1.492(6) . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.390(7) . ? C16 C17 1.404(7) . ? C17 C18 1.379(7) . ? C17 H17 0.9300 . ? C18 C19 1.361(8) . ? C18 H18 0.9300 . ? C19 C20 1.382(7) . ? C19 H19 0.9300 . ? C20 C21 1.395(6) . ? C20 H20 0.9300 . ? C21 C22 1.507(7) . ? C22 O6 1.249(5) . ? C22 O7 1.260(5) . ? C23 C24 1.286(6) . ? C23 N1 1.359(6) . ? C23 H23 0.9300 . ? C24 N2 1.339(6) . ? C24 H24 0.9300 . ? C25 N2 1.316(6) . ? C25 N1 1.327(6) . ? C25 H25 0.9300 . ? C26 N2 1.479(6) . ? C26 C27 1.516(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.365(8) . ? C27 C29 1.373(7) 2_756 ? C28 C29 1.392(7) . ? C28 H28 0.9300 . ? C29 C27 1.373(7) 2_756 ? C29 H29 0.9300 . ? O2 Zn1 2.031(3) 2_666 ? O4 H4O 0.8200 . ? O6 Zn1 2.073(3) 1_454 ? O7 Zn1 2.063(3) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 O1 102.92(14) . . ? N1 Zn1 O2 97.98(14) . 2_666 ? O1 Zn1 O2 159.09(14) . 2_666 ? N1 Zn1 O7 102.98(14) . 2_565 ? O1 Zn1 O7 86.20(15) . 2_565 ? O2 Zn1 O7 89.57(14) 2_666 2_565 ? N1 Zn1 O6 97.50(14) . 1_656 ? O1 Zn1 O6 87.73(14) . 1_656 ? O2 Zn1 O6 89.14(14) 2_666 1_656 ? O7 Zn1 O6 159.46(13) 2_565 1_656 ? N1 Zn1 Zn1 167.61(12) . 2_666 ? O1 Zn1 Zn1 78.54(10) . 2_666 ? O2 Zn1 Zn1 80.95(10) 2_666 2_666 ? O7 Zn1 Zn1 89.37(9) 2_565 2_666 ? O6 Zn1 Zn1 70.18(9) 1_656 2_666 ? C6 C1 C2 120.0(5) . . ? C6 C1 C7 122.2(5) . . ? C2 C1 C7 117.7(5) . . ? C1 C2 C3 120.2(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 119.4(4) . . ? C4 C3 C8 122.2(4) . . ? C2 C3 C8 118.2(4) . . ? C3 C4 C5 120.5(5) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? O5 C5 C6 115.5(4) . . ? O5 C5 C4 124.5(4) . . ? C6 C5 C4 119.9(4) . . ? C1 C6 C5 119.8(5) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? O3 C7 O4 122.0(6) . . ? O3 C7 C1 120.5(6) . . ? O4 C7 C1 117.4(6) . . ? O2 C8 O1 124.8(4) . . ? O2 C8 C3 118.1(4) . . ? O1 C8 C3 117.0(4) . . ? O5 C9 C10 108.6(4) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C11 C10 C15 118.3(4) . . ? C11 C10 C9 120.9(5) . . ? C15 C10 C9 120.7(5) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C13 121.3(5) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 117.7(4) . . ? C14 C13 C16 121.3(4) . . ? C12 C13 C16 120.9(4) . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C10 C15 C14 121.2(5) . . ? C10 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C21 C16 C17 117.9(4) . . ? C21 C16 C13 123.8(4) . . ? C17 C16 C13 118.2(5) . . ? C18 C17 C16 121.5(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.6(5) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C21 121.2(5) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 119.6(4) . . ? C16 C21 C22 124.0(4) . . ? C20 C21 C22 116.1(4) . . ? O6 C22 O7 124.9(5) . . ? O6 C22 C21 117.9(4) . . ? O7 C22 C21 117.2(4) . . ? C24 C23 N1 113.8(5) . . ? C24 C23 H23 123.1 . . ? N1 C23 H23 123.1 . . ? C23 C24 N2 103.6(4) . . ? C23 C24 H24 128.2 . . ? N2 C24 H24 128.2 . . ? N2 C25 N1 108.9(5) . . ? N2 C25 H25 125.5 . . ? N1 C25 H25 125.5 . . ? N2 C26 C27 109.9(4) . . ? N2 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N2 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C29 119.0(4) . 2_756 ? C28 C27 C26 120.9(5) . . ? C29 C27 C26 120.1(5) 2_756 . ? C27 C28 C29 121.9(5) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C27 C29 C28 119.1(5) 2_756 . ? C27 C29 H29 120.5 2_756 . ? C28 C29 H29 120.5 . . ? C25 N1 C23 103.1(4) . . ? C25 N1 Zn1 128.6(4) . . ? C23 N1 Zn1 127.8(3) . . ? C25 N2 C24 110.5(4) . . ? C25 N2 C26 127.7(4) . . ? C24 N2 C26 121.1(4) . . ? C8 O1 Zn1 129.1(3) . . ? C8 O2 Zn1 124.8(3) . 2_666 ? C7 O4 H4O 109.5 . . ? C5 O5 C9 117.2(4) . . ? C22 O6 Zn1 140.1(3) . 1_454 ? C22 O7 Zn1 114.8(3) . 2_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.5(8) . . . . ? C7 C1 C2 C3 175.9(5) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? C1 C2 C3 C8 -175.0(4) . . . . ? C2 C3 C4 C5 2.3(8) . . . . ? C8 C3 C4 C5 177.6(4) . . . . ? C3 C4 C5 O5 177.6(5) . . . . ? C3 C4 C5 C6 -3.0(8) . . . . ? C2 C1 C6 C5 1.9(8) . . . . ? C7 C1 C6 C5 -176.4(5) . . . . ? O5 C5 C6 C1 -179.7(5) . . . . ? C4 C5 C6 C1 0.8(8) . . . . ? C6 C1 C7 O3 167.6(6) . . . . ? C2 C1 C7 O3 -10.8(8) . . . . ? C6 C1 C7 O4 -10.5(8) . . . . ? C2 C1 C7 O4 171.1(5) . . . . ? C4 C3 C8 O2 -21.7(7) . . . . ? C2 C3 C8 O2 153.6(5) . . . . ? C4 C3 C8 O1 159.9(5) . . . . ? C2 C3 C8 O1 -24.8(7) . . . . ? O5 C9 C10 C11 64.6(7) . . . . ? O5 C9 C10 C15 -118.0(6) . . . . ? C15 C10 C11 C12 -0.7(8) . . . . ? C9 C10 C11 C12 176.8(5) . . . . ? C10 C11 C12 C13 0.6(9) . . . . ? C11 C12 C13 C14 -0.5(8) . . . . ? C11 C12 C13 C16 -176.8(5) . . . . ? C12 C13 C14 C15 0.6(8) . . . . ? C16 C13 C14 C15 176.8(5) . . . . ? C11 C10 C15 C14 0.7(8) . . . . ? C9 C10 C15 C14 -176.7(5) . . . . ? C13 C14 C15 C10 -0.7(8) . . . . ? C14 C13 C16 C21 41.2(7) . . . . ? C12 C13 C16 C21 -142.7(5) . . . . ? C14 C13 C16 C17 -135.1(5) . . . . ? C12 C13 C16 C17 41.1(7) . . . . ? C21 C16 C17 C18 -0.7(7) . . . . ? C13 C16 C17 C18 175.7(5) . . . . ? C16 C17 C18 C19 -1.5(8) . . . . ? C17 C18 C19 C20 1.2(9) . . . . ? C18 C19 C20 C21 1.3(9) . . . . ? C17 C16 C21 C20 3.1(7) . . . . ? C13 C16 C21 C20 -173.1(5) . . . . ? C17 C16 C21 C22 -170.7(4) . . . . ? C13 C16 C21 C22 13.1(7) . . . . ? C19 C20 C21 C16 -3.5(8) . . . . ? C19 C20 C21 C22 170.8(5) . . . . ? C16 C21 C22 O6 38.2(7) . . . . ? C20 C21 C22 O6 -135.8(5) . . . . ? C16 C21 C22 O7 -144.3(5) . . . . ? C20 C21 C22 O7 41.7(6) . . . . ? N1 C23 C24 N2 -0.9(5) . . . . ? N2 C26 C27 C28 -65.9(6) . . . . ? N2 C26 C27 C29 112.3(5) . . . 2_756 ? C29 C27 C28 C29 -0.2(9) 2_756 . . . ? C26 C27 C28 C29 178.0(5) . . . . ? C27 C28 C29 C27 0.2(9) . . . 2_756 ? N2 C25 N1 C23 0.1(5) . . . . ? N2 C25 N1 Zn1 172.9(3) . . . . ? C24 C23 N1 C25 0.5(5) . . . . ? C24 C23 N1 Zn1 -172.3(3) . . . . ? O1 Zn1 N1 C25 46.6(4) . . . . ? O2 Zn1 N1 C25 -133.9(4) 2_666 . . . ? O7 Zn1 N1 C25 -42.5(4) 2_565 . . . ? O6 Zn1 N1 C25 135.9(4) 1_656 . . . ? Zn1 Zn1 N1 C25 142.0(4) 2_666 . . . ? O1 Zn1 N1 C23 -142.4(4) . . . . ? O2 Zn1 N1 C23 37.2(4) 2_666 . . . ? O7 Zn1 N1 C23 128.6(4) 2_565 . . . ? O6 Zn1 N1 C23 -53.0(4) 1_656 . . . ? Zn1 Zn1 N1 C23 -46.9(7) 2_666 . . . ? N1 C25 N2 C24 -0.6(5) . . . . ? N1 C25 N2 C26 -171.0(4) . . . . ? C23 C24 N2 C25 0.9(5) . . . . ? C23 C24 N2 C26 172.0(4) . . . . ? C27 C26 N2 C25 83.2(6) . . . . ? C27 C26 N2 C24 -86.2(5) . . . . ? O2 C8 O1 Zn1 -11.4(8) . . . . ? C3 C8 O1 Zn1 166.9(3) . . . . ? N1 Zn1 O1 C8 169.0(4) . . . . ? O2 Zn1 O1 C8 -9.8(7) 2_666 . . . ? O7 Zn1 O1 C8 -88.6(4) 2_565 . . . ? O6 Zn1 O1 C8 71.8(4) 1_656 . . . ? Zn1 Zn1 O1 C8 1.6(4) 2_666 . . . ? O1 C8 O2 Zn1 17.5(7) . . . 2_666 ? C3 C8 O2 Zn1 -160.8(3) . . . 2_666 ? C6 C5 O5 C9 177.3(5) . . . . ? C4 C5 O5 C9 -3.3(8) . . . . ? C10 C9 O5 C5 -176.4(5) . . . . ? O7 C22 O6 Zn1 -9.0(8) . . . 1_454 ? C21 C22 O6 Zn1 168.3(3) . . . 1_454 ? O6 C22 O7 Zn1 9.9(6) . . . 2_565 ? C21 C22 O7 Zn1 -167.4(3) . . . 2_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4O O1W 0.82 2.07 2.851(7) 157.8 2_655 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.934 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 938339' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound-8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H58 N8 O18 Zn3' _chemical_formula_sum 'C72 H58 N8 O18 Zn3' _chemical_formula_weight 1519.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.2960(10) _cell_length_b 10.9930(4) _cell_length_c 27.0310(9) _cell_angle_alpha 90 _cell_angle_beta 103.730(4) _cell_angle_gamma 90 _cell_volume 6724.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3452 _cell_measurement_theta_min 2.9378 _cell_measurement_theta_max 29.1591 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6908 _exptl_absorpt_correction_T_max 0.7406 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.2375 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12580 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5912 _reflns_number_gt 4315 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For O1W and C26', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. For C24, C34, N2 and N4, some anisotropic displacement ellipsoids were rather elongated which led us to use the DELU restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+6.8477P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5912 _refine_ls_number_parameters 465 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.28416(2) 0.18562(4) 0.046403(16) 0.02986(16) Uani 1 1 d . . . Zn2 Zn 0.5000 0.34928(6) -0.2500 0.0406(2) Uani 1 2 d S . . C1 C 0.36986(17) 0.1523(3) -0.07785(15) 0.0314(9) Uani 1 1 d . . . C2 C 0.38283(17) 0.2245(4) -0.11521(14) 0.0324(9) Uani 1 1 d . . . H2 H 0.3622 0.2965 -0.1247 0.039 Uiso 1 1 calc R . . C3 C 0.42744(18) 0.1890(4) -0.13897(14) 0.0334(9) Uani 1 1 d . . . C4 C 0.45533(18) 0.0793(4) -0.12694(15) 0.0366(10) Uani 1 1 d . . . H4 H 0.4843 0.0549 -0.1433 0.044 Uiso 1 1 calc R . . C5 C 0.44053(19) 0.0048(4) -0.09064(16) 0.0393(10) Uani 1 1 d . . . C6 C 0.39873(18) 0.0425(4) -0.06477(16) 0.0378(10) Uani 1 1 d . . . H6 H 0.3903 -0.0053 -0.0390 0.045 Uiso 1 1 calc R . . C7 C 0.32446(18) 0.1904(3) -0.05032(16) 0.0346(9) Uani 1 1 d . . . C8 C 0.4422(2) 0.2718(4) -0.17868(15) 0.0406(10) Uani 1 1 d . . . C9 C 0.4491(2) -0.1914(4) -0.0500(2) 0.0534(13) Uani 1 1 d . . . H9A H 0.4076 -0.2099 -0.0636 0.064 Uiso 1 1 calc R . . H9B H 0.4542 -0.1602 -0.0156 0.064 Uiso 1 1 calc R . . C10 C 0.4862(2) -0.3018(4) -0.05034(18) 0.0437(11) Uani 1 1 d . . . C11 C 0.4781(2) -0.3754(4) -0.09301(19) 0.0531(12) Uani 1 1 d . . . H11 H 0.4465 -0.3610 -0.1207 0.064 Uiso 1 1 calc R . . C12 C 0.5165(2) -0.4698(4) -0.09480(17) 0.0472(12) Uani 1 1 d . . . H12 H 0.5107 -0.5179 -0.1239 0.057 Uiso 1 1 calc R . . C13 C 0.56375(19) -0.4942(3) -0.05374(16) 0.0367(10) Uani 1 1 d . . . C14 C 0.57000(19) -0.4240(4) -0.01001(16) 0.0403(10) Uani 1 1 d . . . H14 H 0.6001 -0.4412 0.0185 0.048 Uiso 1 1 calc R . . C15 C 0.5316(2) -0.3286(4) -0.00868(18) 0.0437(11) Uani 1 1 d . . . H15 H 0.5365 -0.2818 0.0207 0.052 Uiso 1 1 calc R . . C16 C 0.6053(2) -0.5937(4) -0.05692(15) 0.0380(10) Uani 1 1 d . . . C17 C 0.5823(2) -0.7073(4) -0.07551(18) 0.0508(12) Uani 1 1 d . . . H17 H 0.5416 -0.7183 -0.0850 0.061 Uiso 1 1 calc R . . C18 C 0.6189(3) -0.8023(4) -0.0799(2) 0.0716(17) Uani 1 1 d . . . H18 H 0.6029 -0.8774 -0.0917 0.086 Uiso 1 1 calc R . . C19 C 0.6781(3) -0.7873(4) -0.0672(2) 0.0785(19) Uani 1 1 d . . . H19 H 0.7025 -0.8514 -0.0715 0.094 Uiso 1 1 calc R . . C20 C 0.7029(2) -0.6771(4) -0.04780(19) 0.0572(14) Uani 1 1 d . . . H20 H 0.7438 -0.6686 -0.0382 0.069 Uiso 1 1 calc R . . C21 C 0.6668(2) -0.5797(3) -0.04273(15) 0.0381(10) Uani 1 1 d . . . C22 C 0.69686(18) -0.4613(4) -0.02339(16) 0.0343(10) Uani 1 1 d . . . C23 C 0.4018(2) 0.1494(4) 0.12089(17) 0.0504(12) Uani 1 1 d . . . H23 H 0.4211 0.1824 0.0975 0.060 Uiso 1 1 calc R . . C24 C 0.42966(18) 0.1142(4) 0.16608(16) 0.0452(11) Uani 1 1 d U . . H24 H 0.4700 0.1163 0.1808 0.054 Uiso 1 1 calc R . . C25 C 0.3350(2) 0.0864(5) 0.15327(17) 0.0516(13) Uani 1 1 d . . . H25 H 0.2986 0.0646 0.1591 0.062 Uiso 1 1 calc R . . C26 C 0.4041(7) 0.0520(14) 0.2436(5) 0.056(4) Uani 0.50 1 d P . . C26' C 0.4014(8) -0.0103(15) 0.2319(6) 0.074(5) Uani 0.50 1 d PU . . C27 C 0.3493(3) 0.0121(9) 0.2612(2) 0.083(2) Uani 1 1 d . . . C28 C 0.3209(3) -0.0974(8) 0.2587(2) 0.087(2) Uani 1 1 d . . . H28 H 0.3311 -0.1607 0.2396 0.104 Uiso 1 1 calc R . . C29 C 0.2764(3) -0.1141(6) 0.2849(2) 0.0785(18) Uani 1 1 d . . . H29 H 0.2573 -0.1888 0.2830 0.094 Uiso 1 1 calc R . . C30 C 0.2604(3) -0.0230(7) 0.31303(19) 0.0690(17) Uani 1 1 d . . . C31 C 0.2894(3) 0.0871(8) 0.3146(2) 0.094(2) Uani 1 1 d . . . H31 H 0.2789 0.1514 0.3330 0.112 Uiso 1 1 calc R . . C32 C 0.3341(3) 0.1034(8) 0.2891(3) 0.096(2) Uani 1 1 d . . . H32 H 0.3536 0.1776 0.2912 0.115 Uiso 1 1 calc R . . C33 C 0.5781(3) 0.5738(5) -0.2385(3) 0.0754(17) Uani 1 1 d . . . H33 H 0.5510 0.6137 -0.2642 0.090 Uiso 1 1 calc R . . C34 C 0.6306(3) 0.6137(5) -0.2198(3) 0.0720(15) Uani 1 1 d U . . H34 H 0.6479 0.6842 -0.2285 0.086 Uiso 1 1 calc R . . C35 C 0.6153(3) 0.4441(6) -0.1839(2) 0.0675(16) Uani 1 1 d . . . H35 H 0.6223 0.3765 -0.1626 0.081 Uiso 1 1 calc R . . C36 C 0.7167(3) 0.5409(7) -0.1552(2) 0.096(2) Uani 1 1 d . . . H36A H 0.7238 0.4805 -0.1282 0.116 Uiso 1 1 calc R . . H36B H 0.7227 0.6206 -0.1394 0.116 Uiso 1 1 calc R . . N1 N 0.34298(15) 0.1342(3) 0.11071(12) 0.0352(8) Uani 1 1 d . . . N2 N 0.38618(17) 0.0743(4) 0.18624(14) 0.0587(11) Uani 1 1 d U . . N3 N 0.5655(2) 0.4668(4) -0.21699(16) 0.0570(11) Uani 1 1 d . . . N4 N 0.6544(2) 0.5308(5) -0.18498(18) 0.0722(13) Uani 1 1 d U . . O1 O 0.33023(14) 0.1518(3) -0.00576(11) 0.0454(8) Uani 1 1 d . . . O2 O 0.28387(13) 0.2581(3) -0.07399(11) 0.0436(7) Uani 1 1 d . . . O3 O 0.48232(14) 0.2363(3) -0.19984(12) 0.0530(8) Uani 1 1 d . . . O4 O 0.41660(19) 0.3690(3) -0.18813(15) 0.0772(12) Uani 1 1 d . . . O5 O 0.46960(15) -0.1046(3) -0.08180(13) 0.0596(10) Uani 1 1 d . . . O6 O 0.68574(13) -0.3690(2) -0.05111(11) 0.0387(7) Uani 1 1 d . . . O7 O 0.73323(14) -0.4654(2) 0.01951(11) 0.0454(8) Uani 1 1 d . . . O1W O 0.3108(3) 0.4776(6) -0.1828(3) 0.155(2) Uani 1 1 d U . . O2W O 0.1957(3) -0.1252(7) 0.0998(3) 0.183(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0349(3) 0.0330(3) 0.0242(2) 0.00383(19) 0.01201(19) 0.0070(2) Zn2 0.0453(5) 0.0454(4) 0.0370(4) 0.000 0.0216(3) 0.000 C1 0.030(2) 0.036(2) 0.031(2) -0.0083(18) 0.0101(17) -0.0023(17) C2 0.032(2) 0.039(2) 0.028(2) -0.0029(18) 0.0085(17) 0.0002(18) C3 0.037(2) 0.041(2) 0.0242(19) -0.0067(18) 0.0106(17) -0.0057(19) C4 0.032(2) 0.046(2) 0.036(2) -0.005(2) 0.0176(19) 0.0005(19) C5 0.039(3) 0.039(2) 0.045(2) 0.000(2) 0.020(2) 0.0048(19) C6 0.042(3) 0.040(2) 0.037(2) 0.0005(19) 0.020(2) 0.0006(19) C7 0.038(3) 0.030(2) 0.041(2) -0.007(2) 0.018(2) -0.0037(19) C8 0.046(3) 0.047(3) 0.031(2) -0.007(2) 0.014(2) -0.005(2) C9 0.058(3) 0.048(3) 0.066(3) 0.015(2) 0.038(3) 0.010(2) C10 0.045(3) 0.040(2) 0.054(3) 0.005(2) 0.027(2) 0.003(2) C11 0.047(3) 0.063(3) 0.048(3) 0.007(2) 0.008(2) 0.013(2) C12 0.050(3) 0.048(3) 0.039(2) -0.004(2) 0.002(2) 0.008(2) C13 0.041(3) 0.031(2) 0.040(2) 0.0025(19) 0.014(2) -0.0045(18) C14 0.041(3) 0.043(3) 0.037(2) 0.001(2) 0.009(2) 0.001(2) C15 0.046(3) 0.040(2) 0.049(3) -0.011(2) 0.018(2) -0.007(2) C16 0.047(3) 0.032(2) 0.032(2) 0.0040(18) 0.004(2) -0.0001(19) C17 0.059(3) 0.032(2) 0.056(3) -0.004(2) 0.004(2) -0.006(2) C18 0.082(4) 0.033(3) 0.085(4) -0.012(3) -0.010(3) 0.003(3) C19 0.092(5) 0.035(3) 0.094(4) -0.017(3) -0.005(4) 0.023(3) C20 0.050(3) 0.044(3) 0.069(3) -0.009(2) -0.003(3) 0.015(2) C21 0.053(3) 0.029(2) 0.031(2) 0.0017(18) 0.006(2) 0.0077(19) C22 0.035(2) 0.033(2) 0.040(2) -0.002(2) 0.018(2) 0.0077(18) C23 0.039(3) 0.073(3) 0.042(3) 0.009(2) 0.016(2) 0.004(2) C24 0.021(2) 0.082(3) 0.031(2) 0.019(2) 0.0008(16) 0.011(2) C25 0.027(3) 0.082(3) 0.047(3) 0.026(3) 0.010(2) 0.011(2) C26 0.051(7) 0.090(10) 0.028(6) 0.031(7) 0.007(5) 0.021(8) C26' 0.075(8) 0.097(9) 0.057(8) 0.036(7) 0.032(6) 0.015(7) C27 0.055(4) 0.146(7) 0.045(3) 0.052(4) 0.007(3) 0.012(4) C28 0.070(5) 0.142(7) 0.050(3) 0.021(4) 0.019(3) 0.049(4) C29 0.064(4) 0.103(5) 0.070(4) 0.033(4) 0.017(3) 0.019(3) C30 0.056(4) 0.115(5) 0.038(3) 0.035(3) 0.015(3) 0.023(4) C31 0.100(6) 0.127(6) 0.055(4) 0.017(4) 0.020(4) 0.029(5) C32 0.089(5) 0.117(6) 0.081(5) 0.033(5) 0.016(4) -0.003(4) C33 0.075(4) 0.058(3) 0.103(5) -0.002(3) 0.041(4) -0.006(3) C34 0.061(4) 0.054(3) 0.112(5) -0.028(2) 0.042(3) -0.036(3) C35 0.075(4) 0.090(4) 0.045(3) -0.012(3) 0.031(3) -0.014(3) C36 0.071(4) 0.164(7) 0.061(4) -0.053(4) 0.030(3) -0.041(4) N1 0.040(2) 0.0381(19) 0.0291(18) 0.0085(15) 0.0119(15) 0.0092(16) N2 0.037(2) 0.097(3) 0.045(2) 0.035(2) 0.0150(18) 0.018(2) N3 0.057(3) 0.070(3) 0.051(2) -0.018(2) 0.028(2) -0.013(2) N4 0.069(3) 0.098(4) 0.058(3) -0.037(2) 0.032(2) -0.026(3) O1 0.056(2) 0.0509(18) 0.0373(17) -0.0022(14) 0.0278(15) 0.0076(14) O2 0.0420(18) 0.0486(18) 0.0475(17) 0.0020(15) 0.0254(15) 0.0082(15) O3 0.061(2) 0.062(2) 0.0467(18) 0.0075(16) 0.0331(16) 0.0034(16) O4 0.109(3) 0.062(2) 0.080(3) 0.027(2) 0.061(2) 0.025(2) O5 0.068(2) 0.0498(19) 0.079(2) 0.0207(17) 0.053(2) 0.0257(17) O6 0.0448(18) 0.0289(15) 0.0438(17) 0.0024(14) 0.0130(14) 0.0008(13) O7 0.053(2) 0.0398(17) 0.0393(17) -0.0033(13) 0.0038(15) -0.0035(14) O1W 0.155(3) 0.157(2) 0.154(2) 0.0021(10) 0.0376(11) 0.0041(10) O2W 0.183(3) 0.183(3) 0.183(3) 0.0014(10) 0.0449(12) 0.0005(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.999(3) . ? Zn1 O2 2.003(3) 7 ? Zn1 N1 2.022(3) . ? Zn1 O7 2.070(3) 3_455 ? Zn1 O6 2.129(3) 5_655 ? Zn1 Zn1 2.9891(8) 7 ? Zn2 O3 1.953(3) 2_654 ? Zn2 O3 1.953(3) . ? Zn2 N3 2.036(4) . ? Zn2 N3 2.036(4) 2_654 ? C1 C2 1.373(5) . ? C1 C6 1.386(6) . ? C1 C7 1.491(5) . ? C2 C3 1.401(5) . ? C2 H2 0.9300 . ? C3 C4 1.372(6) . ? C3 C8 1.509(6) . ? C4 C5 1.383(6) . ? C4 H4 0.9300 . ? C5 O5 1.372(5) . ? C5 C6 1.390(6) . ? C6 H6 0.9300 . ? C7 O2 1.253(5) . ? C7 O1 1.254(5) . ? C8 O4 1.221(5) . ? C8 O3 1.267(5) . ? C9 O5 1.440(5) . ? C9 C10 1.492(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.381(6) . ? C10 C11 1.384(7) . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 C13 1.391(6) . ? C12 H12 0.9300 . ? C13 C14 1.390(6) . ? C13 C16 1.477(6) . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.401(6) . ? C16 C17 1.405(6) . ? C17 C18 1.372(7) . ? C17 H17 0.9300 . ? C18 C19 1.349(8) . ? C18 H18 0.9300 . ? C19 C20 1.391(7) . ? C19 H19 0.9300 . ? C20 C21 1.388(6) . ? C20 H20 0.9300 . ? C21 C22 1.511(6) . ? C22 O6 1.251(5) . ? C22 O7 1.264(5) . ? C23 C24 1.299(6) . ? C23 N1 1.343(6) . ? C23 H23 0.9300 . ? C24 N2 1.333(6) . ? C24 H24 0.9300 . ? C25 N2 1.315(5) . ? C25 N1 1.317(5) . ? C25 H25 0.9300 . ? C26 C26' 0.750(18) . ? C26 N2 1.526(13) . ? C26 C27 1.528(17) . ? C26' N2 1.519(16) . ? C26' C27 1.617(19) . ? C27 C32 1.353(10) . ? C27 C28 1.367(10) . ? C28 C29 1.400(9) . ? C28 H28 0.9300 . ? C29 C30 1.361(9) . ? C29 H29 0.9300 . ? C30 C31 1.383(9) . ? C30 C36 1.493(8) 8_456 ? C31 C32 1.390(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.284(8) . ? C33 N3 1.373(7) . ? C33 H33 0.9300 . ? C34 N4 1.333(8) . ? C34 H34 0.9300 . ? C35 N3 1.311(7) . ? C35 N4 1.324(7) . ? C35 H35 0.9300 . ? C36 N4 1.487(7) . ? C36 C30 1.493(8) 8 ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? O2 Zn1 2.003(3) 7 ? O6 Zn1 2.129(3) 5_655 ? O7 Zn1 2.070(3) 3_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 157.63(12) . 7 ? O1 Zn1 N1 100.76(13) . . ? O2 Zn1 N1 101.59(13) 7 . ? O1 Zn1 O7 87.83(12) . 3_455 ? O2 Zn1 O7 86.56(12) 7 3_455 ? N1 Zn1 O7 107.03(12) . 3_455 ? O1 Zn1 O6 89.66(11) . 5_655 ? O2 Zn1 O6 87.92(11) 7 5_655 ? N1 Zn1 O6 93.84(12) . 5_655 ? O7 Zn1 O6 159.09(11) 3_455 5_655 ? O1 Zn1 Zn1 76.36(9) . 7 ? O2 Zn1 Zn1 81.69(9) 7 7 ? N1 Zn1 Zn1 166.19(10) . 7 ? O7 Zn1 Zn1 86.47(8) 3_455 7 ? O6 Zn1 Zn1 72.77(8) 5_655 7 ? O3 Zn2 O3 101.04(19) 2_654 . ? O3 Zn2 N3 116.63(14) 2_654 . ? O3 Zn2 N3 111.02(16) . . ? O3 Zn2 N3 111.02(16) 2_654 2_654 ? O3 Zn2 N3 116.63(14) . 2_654 ? N3 Zn2 N3 101.2(3) . 2_654 ? C2 C1 C6 120.9(4) . . ? C2 C1 C7 120.7(4) . . ? C6 C1 C7 118.4(4) . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 C8 121.6(4) . . ? C2 C3 C8 118.5(4) . . ? C3 C4 C5 120.3(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? O5 C5 C4 116.5(4) . . ? O5 C5 C6 123.3(4) . . ? C4 C5 C6 120.1(4) . . ? C1 C6 C5 119.1(4) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O2 C7 O1 126.0(4) . . ? O2 C7 C1 116.8(4) . . ? O1 C7 C1 117.2(4) . . ? O4 C8 O3 123.5(4) . . ? O4 C8 C3 119.6(4) . . ? O3 C8 C3 116.9(4) . . ? O5 C9 C10 105.1(3) . . ? O5 C9 H9A 110.7 . . ? C10 C9 H9A 110.7 . . ? O5 C9 H9B 110.7 . . ? C10 C9 H9B 110.7 . . ? H9A C9 H9B 108.8 . . ? C15 C10 C11 118.8(4) . . ? C15 C10 C9 120.0(4) . . ? C11 C10 C9 121.1(4) . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 118.3(4) . . ? C14 C13 C16 121.5(4) . . ? C12 C13 C16 120.1(4) . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C10 C15 C14 121.0(4) . . ? C10 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C21 C16 C17 118.3(4) . . ? C21 C16 C13 123.1(4) . . ? C17 C16 C13 118.6(4) . . ? C18 C17 C16 121.0(5) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C16 119.5(4) . . ? C20 C21 C22 117.2(4) . . ? C16 C21 C22 123.2(4) . . ? O6 C22 O7 125.2(4) . . ? O6 C22 C21 118.6(4) . . ? O7 C22 C21 116.2(4) . . ? C24 C23 N1 114.4(4) . . ? C24 C23 H23 122.8 . . ? N1 C23 H23 122.8 . . ? C23 C24 N2 103.0(4) . . ? C23 C24 H24 128.5 . . ? N2 C24 H24 128.5 . . ? N2 C25 N1 109.9(4) . . ? N2 C25 H25 125.1 . . ? N1 C25 H25 125.1 . . ? C26' C26 N2 75(2) . . ? C26' C26 C27 83(2) . . ? N2 C26 C27 108.4(9) . . ? C26 C26' N2 76.2(19) . . ? C26 C26' C27 70(2) . . ? N2 C26' C27 104.3(10) . . ? C32 C27 C28 119.5(7) . . ? C32 C27 C26 108.1(9) . . ? C28 C27 C26 131.9(9) . . ? C32 C27 C26' 135.5(10) . . ? C28 C27 C26' 104.6(9) . . ? C26 C27 C26' 27.4(7) . . ? C27 C28 C29 119.9(7) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 121.3(7) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 117.7(6) . . ? C29 C30 C36 122.6(7) . 8_456 ? C31 C30 C36 119.5(7) . 8_456 ? C30 C31 C32 121.0(7) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C27 C32 C31 120.6(8) . . ? C27 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 N3 113.9(6) . . ? C34 C33 H33 123.0 . . ? N3 C33 H33 123.0 . . ? C33 C34 N4 104.0(5) . . ? C33 C34 H34 128.0 . . ? N4 C34 H34 128.0 . . ? N3 C35 N4 110.5(6) . . ? N3 C35 H35 124.8 . . ? N4 C35 H35 124.8 . . ? N4 C36 C30 112.9(4) . 8 ? N4 C36 H36A 109.0 . . ? C30 C36 H36A 109.0 8 . ? N4 C36 H36B 109.0 . . ? C30 C36 H36B 109.0 8 . ? H36A C36 H36B 107.8 . . ? C25 N1 C23 102.7(4) . . ? C25 N1 Zn1 130.9(3) . . ? C23 N1 Zn1 126.3(3) . . ? C25 N2 C24 110.1(4) . . ? C25 N2 C26' 127.8(8) . . ? C24 N2 C26' 118.7(8) . . ? C25 N2 C26 133.6(7) . . ? C24 N2 C26 114.6(7) . . ? C26' N2 C26 28.5(7) . . ? C35 N3 C33 102.0(5) . . ? C35 N3 Zn2 128.9(4) . . ? C33 N3 Zn2 124.8(4) . . ? C35 N4 C34 109.5(5) . . ? C35 N4 C36 129.0(6) . . ? C34 N4 C36 121.4(5) . . ? C7 O1 Zn1 131.4(3) . . ? C7 O2 Zn1 124.1(3) . 7 ? C8 O3 Zn2 114.6(3) . . ? C5 O5 C9 117.7(3) . . ? C22 O6 Zn1 135.6(3) . 5_655 ? C22 O7 Zn1 119.8(3) . 3_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.5(6) . . . . ? C7 C1 C2 C3 177.3(3) . . . . ? C1 C2 C3 C4 3.8(6) . . . . ? C1 C2 C3 C8 -178.0(3) . . . . ? C2 C3 C4 C5 -1.4(6) . . . . ? C8 C3 C4 C5 -179.5(4) . . . . ? C3 C4 C5 O5 178.5(4) . . . . ? C3 C4 C5 C6 -2.3(6) . . . . ? C2 C1 C6 C5 -1.2(6) . . . . ? C7 C1 C6 C5 179.0(4) . . . . ? O5 C5 C6 C1 -177.3(4) . . . . ? C4 C5 C6 C1 3.6(6) . . . . ? C2 C1 C7 O2 27.9(5) . . . . ? C6 C1 C7 O2 -152.2(4) . . . . ? C2 C1 C7 O1 -152.2(4) . . . . ? C6 C1 C7 O1 27.7(5) . . . . ? C4 C3 C8 O4 -179.7(4) . . . . ? C2 C3 C8 O4 2.2(6) . . . . ? C4 C3 C8 O3 -1.1(6) . . . . ? C2 C3 C8 O3 -179.2(4) . . . . ? O5 C9 C10 C15 103.8(5) . . . . ? O5 C9 C10 C11 -72.7(6) . . . . ? C15 C10 C11 C12 -3.3(7) . . . . ? C9 C10 C11 C12 173.3(4) . . . . ? C10 C11 C12 C13 0.7(7) . . . . ? C11 C12 C13 C14 2.5(7) . . . . ? C11 C12 C13 C16 -178.3(4) . . . . ? C12 C13 C14 C15 -3.1(6) . . . . ? C16 C13 C14 C15 177.7(4) . . . . ? C11 C10 C15 C14 2.6(7) . . . . ? C9 C10 C15 C14 -173.9(4) . . . . ? C13 C14 C15 C10 0.6(7) . . . . ? C14 C13 C16 C21 -48.6(6) . . . . ? C12 C13 C16 C21 132.3(5) . . . . ? C14 C13 C16 C17 132.1(4) . . . . ? C12 C13 C16 C17 -47.1(6) . . . . ? C21 C16 C17 C18 -0.3(7) . . . . ? C13 C16 C17 C18 179.1(5) . . . . ? C16 C17 C18 C19 -1.2(9) . . . . ? C17 C18 C19 C20 2.3(10) . . . . ? C18 C19 C20 C21 -2.0(9) . . . . ? C19 C20 C21 C16 0.5(7) . . . . ? C19 C20 C21 C22 -177.6(5) . . . . ? C17 C16 C21 C20 0.6(6) . . . . ? C13 C16 C21 C20 -178.7(4) . . . . ? C17 C16 C21 C22 178.5(4) . . . . ? C13 C16 C21 C22 -0.8(6) . . . . ? C20 C21 C22 O6 120.1(4) . . . . ? C16 C21 C22 O6 -57.9(6) . . . . ? C20 C21 C22 O7 -57.6(5) . . . . ? C16 C21 C22 O7 124.5(4) . . . . ? N1 C23 C24 N2 -0.2(6) . . . . ? C27 C26 C26' N2 111.2(5) . . . . ? N2 C26 C26' C27 -111.2(5) . . . . ? C26' C26 C27 C32 178.5(19) . . . . ? N2 C26 C27 C32 -109.7(9) . . . . ? C26' C26 C27 C28 7(2) . . . . ? N2 C26 C27 C28 79.3(11) . . . . ? N2 C26 C27 C26' 72(2) . . . . ? C26 C26' C27 C32 -2(3) . . . . ? N2 C26' C27 C32 -71.2(14) . . . . ? C26 C26' C27 C28 -174.3(18) . . . . ? N2 C26' C27 C28 116.6(9) . . . . ? N2 C26' C27 C26 -69.2(18) . . . . ? C32 C27 C28 C29 0.1(9) . . . . ? C26 C27 C28 C29 170.2(8) . . . . ? C26' C27 C28 C29 173.8(8) . . . . ? C27 C28 C29 C30 0.1(9) . . . . ? C28 C29 C30 C31 0.5(8) . . . . ? C28 C29 C30 C36 -174.8(5) . . . 8_456 ? C29 C30 C31 C32 -1.2(9) . . . . ? C36 C30 C31 C32 174.2(5) 8_456 . . . ? C28 C27 C32 C31 -0.8(10) . . . . ? C26 C27 C32 C31 -173.1(7) . . . . ? C26' C27 C32 C31 -172.1(10) . . . . ? C30 C31 C32 C27 1.4(10) . . . . ? N3 C33 C34 N4 0.6(7) . . . . ? N2 C25 N1 C23 -0.1(5) . . . . ? N2 C25 N1 Zn1 -176.3(3) . . . . ? C24 C23 N1 C25 0.2(6) . . . . ? C24 C23 N1 Zn1 176.6(3) . . . . ? O1 Zn1 N1 C25 -148.1(4) . . . . ? O2 Zn1 N1 C25 32.9(4) 7 . . . ? O7 Zn1 N1 C25 -57.0(4) 3_455 . . . ? O6 Zn1 N1 C25 121.6(4) 5_655 . . . ? Zn1 Zn1 N1 C25 135.4(4) 7 . . . ? O1 Zn1 N1 C23 36.6(4) . . . . ? O2 Zn1 N1 C23 -142.4(3) 7 . . . ? O7 Zn1 N1 C23 127.6(3) 3_455 . . . ? O6 Zn1 N1 C23 -53.8(4) 5_655 . . . ? Zn1 Zn1 N1 C23 -39.9(6) 7 . . . ? N1 C25 N2 C24 0.0(6) . . . . ? N1 C25 N2 C26' -158.5(9) . . . . ? N1 C25 N2 C26 164.3(9) . . . . ? C23 C24 N2 C25 0.1(6) . . . . ? C23 C24 N2 C26' 160.8(8) . . . . ? C23 C24 N2 C26 -167.5(7) . . . . ? C26 C26' N2 C25 -114(2) . . . . ? C27 C26' N2 C25 -49.3(13) . . . . ? C26 C26' N2 C24 89(2) . . . . ? C27 C26' N2 C24 153.7(7) . . . . ? C27 C26' N2 C26 64(2) . . . . ? C26' C26 N2 C25 91(2) . . . . ? C27 C26 N2 C25 13.9(15) . . . . ? C26' C26 N2 C24 -105(2) . . . . ? C27 C26 N2 C24 177.6(7) . . . . ? C27 C26 N2 C26' -77(2) . . . . ? N4 C35 N3 C33 0.6(6) . . . . ? N4 C35 N3 Zn2 157.9(3) . . . . ? C34 C33 N3 C35 -0.8(6) . . . . ? C34 C33 N3 Zn2 -159.3(4) . . . . ? O3 Zn2 N3 C35 -70.9(4) 2_654 . . . ? O3 Zn2 N3 C35 44.1(4) . . . . ? N3 Zn2 N3 C35 168.5(5) 2_654 . . . ? O3 Zn2 N3 C33 81.7(4) 2_654 . . . ? O3 Zn2 N3 C33 -163.4(4) . . . . ? N3 Zn2 N3 C33 -38.9(4) 2_654 . . . ? N3 C35 N4 C34 -0.3(6) . . . . ? N3 C35 N4 C36 -178.3(5) . . . . ? C33 C34 N4 C35 -0.2(6) . . . . ? C33 C34 N4 C36 178.0(5) . . . . ? C30 C36 N4 C35 109.6(7) 8 . . . ? C30 C36 N4 C34 -68.1(8) 8 . . . ? O2 C7 O1 Zn1 -4.2(6) . . . . ? C1 C7 O1 Zn1 175.9(3) . . . . ? O2 Zn1 O1 C7 17.3(6) 7 . . . ? N1 Zn1 O1 C7 -160.2(4) . . . . ? O7 Zn1 O1 C7 92.8(4) 3_455 . . . ? O6 Zn1 O1 C7 -66.4(4) 5_655 . . . ? Zn1 Zn1 O1 C7 6.0(3) 7 . . . ? O1 C7 O2 Zn1 -3.1(6) . . . 7 ? C1 C7 O2 Zn1 176.9(2) . . . 7 ? O4 C8 O3 Zn2 -0.6(6) . . . . ? C3 C8 O3 Zn2 -179.1(3) . . . . ? O3 Zn2 O3 C8 -144.8(3) 2_654 . . . ? N3 Zn2 O3 C8 90.9(3) . . . . ? N3 Zn2 O3 C8 -24.3(4) 2_654 . . . ? C4 C5 O5 C9 -171.0(4) . . . . ? C6 C5 O5 C9 9.9(7) . . . . ? C10 C9 O5 C5 176.4(4) . . . . ? O7 C22 O6 Zn1 0.6(6) . . . 5_655 ? C21 C22 O6 Zn1 -176.9(3) . . . 5_655 ? O6 C22 O7 Zn1 -4.4(5) . . . 3_545 ? C21 C22 O7 Zn1 173.1(3) . . . 3_545 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.898 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.071 #=========================END _database_code_depnum_ccdc_archive 'CCDC 938340'